CN112362595A - Method for testing content of impurity elements in sponge platinum - Google Patents
Method for testing content of impurity elements in sponge platinum Download PDFInfo
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- CN112362595A CN112362595A CN202011402417.2A CN202011402417A CN112362595A CN 112362595 A CN112362595 A CN 112362595A CN 202011402417 A CN202011402417 A CN 202011402417A CN 112362595 A CN112362595 A CN 112362595A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
Abstract
The invention belongs to the technical field of analysis and test, and particularly discloses a method for testing the content of impurity elements in sponge platinum, which is simple and convenient to operate and high in detection precision. According to the method for testing the content of the impurity elements in the spongy platinum, after the spongy platinum to be tested is manufactured into a sheet sample, the sheet sample is directly tested by adopting a direct-reading spectrometer which is implanted with a standard curve of each impurity element and is verified to be reliable, so that the content of each impurity element is obtained; the whole process is convenient to operate, simple and easy, rapid in detection and lower in detection limit, the spongy platinum with the Pt purity being more than or equal to 99.995% can be detected, and the analysis efficiency and the accuracy of the detection result are greatly improved.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and particularly relates to a method for testing the content of impurity elements in spongy platinum.
Background
In modern industry, platinum is more and more widely used, such as automobile exhaust catalysts, aerospace, microelectronic technology, instrument electronics, medicine, metallurgy, and the like. The reason is that platinum has excellent physical, chemical and electrical properties, but platinum resources are scarce, and the regeneration and recovery of waste materials are extremely important. Sponge platinum is a purified product of recovered platinum and is a raw material for producing various platinum products, and the intrinsic quality of sponge platinum is more and more important.
At present, most of impurities in sponge platinum are detected by a method of dissolving a sample by aqua regia and then detecting the content of the impurity elements by using a plasma emission spectrometer (ICP-OES), but the method is inconvenient to operate and high in danger, and the minimum content of the impurity elements is 5 ppm.
Disclosure of Invention
The invention aims to provide a method for testing the content of impurity elements in sponge platinum, which is simple and convenient to operate and high in detection precision.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for testing the content of impurity elements in the sponge platinum comprises the following steps:
preparing sponge platinum to be tested into a sheet sample;
selecting a direct-reading spectrometer with an impurity element detection channel as a test instrument, selecting 6-8 standard samples with different impurity element contents, measuring the corresponding light intensity values of the impurity elements with different contents by using the direct-reading spectrometer, and implanting the standard curve of the impurity elements established by the direct-reading spectrometer into the direct-reading spectrometer;
step three, measuring the known standard control sample with the content of each impurity element for more than 20 times by adopting a direct-reading spectrometer implanted with a standard curve to obtain the content of each impurity element, taking an average value as a test result, calculating the difference between the test result and a true value and the precision of the test result, if the difference between the test result and the true value and the precision of the test result are in an allowable range, indicating that the direct-reading spectrometer implanted with the standard curve is reliable, otherwise, repeating the step two and the step three;
and step four, testing the sheet sample by using the direct-reading spectrometer verified to be reliable in step three, fixing the sheet sample on an excitation table of the direct-reading spectrometer, exciting 3-5 points on the test sheet sample, and averaging the results to obtain the content of each impurity in the sponge platinum.
Further, in the first step, the granular sponge platinum is pressed into a sheet sample by a stamping die.
Further, the stamping die comprises a top die, a middle die and a bottom die; the middle die is provided with a middle die hole penetrating through the middle die, the top die comprises a top die plate and a pressing part arranged on the lower side of the top die plate and matched with the middle die hole, and the bottom die comprises a bottom die plate and a supporting part arranged on the upper side of the bottom die plate and matched with the middle die hole.
Further, stamping die still includes unloads the appearance die block, the top of unloading the appearance die block be equipped with well mould looks adaptation go up the step hole and set up unload in the appearance die block and with last communicating lower step hole in step hole, the cross section size in lower step hole is greater than the cross section size in well mould hole.
Further, the process of making the sheet sample in the step one is as follows:
a. cleaning each part of the stamping die by using dust-free paper dipped with alcohol for later use;
b. mounting a middle die on a bottom die, and embedding a supporting part from the lower end of a middle die hole; weighing 10-15 g of spongy platinum to be tested with the diameter of less than 3mm, and pouring the spongy platinum into a middle die hole;
c. mounting a top die on the middle die, and embedding a pressure applying part from the upper end of a middle die hole; then, pressing the top die by using pressure equipment, controlling the pressure to be 25-35 Kpa, and continuously pressing for 15-20 s to obtain a sheet sample;
d. taking the middle die containing the sheet sample and the top die from the bottom die together, then installing the middle die on the sample unloading bottom die, and finally applying pressure to the top die to press the sheet sample into the lower step hole and take out the sheet sample;
e. soaking the taken sheet sample in dilute hydrochloric acid for 5-10 min, then taking out and washing with clear water, then washing with absolute ethyl alcohol, and finally drying for later use.
Further, the impurity element includes at least one of Au, Ag, Pd, Rh, Ir, Ru, Al, As, B, Bi, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sb, Si, Sn, Ti, Zn and Zr.
Further, the standard control samples comprise a first type of standard control sample with Pt purity being more than or equal to 99.99% and a second type of standard control sample with Pt purity being more than or equal to 99.9%.
Further, the third step further includes measuring the high-purity sample for more than 10 times by using a direct-reading spectrometer implanted with a standard curve to obtain a test light intensity value of each impurity element, calculating a standard deviation sigma of the light intensity value of each impurity element, and obtaining a detection lower limit of each impurity element according to a formula LOD (log-3 sigma) K; wherein, the Pt purity of the high-purity sample is more than 99.999 percent, and K is the slope of the curve.
Furthermore, in the third step, the lower detection limit of each impurity element is shown in the following table:
| impurity element | Au | Ag | Pd | Rh | Ir | Ru | Al | As | B | Bi |
| Lower detection limit (ppm) | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 1-2 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 |
| Impurity element | Ca | Cd | Co | Cr | Cu | Fe | Mg | Mn | Mo | Ni |
| Lower detection limit (ppm) | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 |
| Impurity element | Pb | Sb | Si | Sn | Ti | Zn | Zr | |||
| Lower detection limit (ppm) | 0.5-1 | 1-2 | 0.5-1 | 1-2 | 0.5-1 | 0.5-1 | 0.5-1 |
。
The invention has the beneficial effects that: according to the method for testing the content of the impurity elements in the spongy platinum, after the spongy platinum to be tested is manufactured into a sheet sample, the sheet sample is directly tested by adopting a direct-reading spectrometer which is implanted with a standard curve of each impurity element and is verified to be reliable, so that the content of each impurity element is obtained; the whole process is convenient to operate, simple and easy, rapid in detection and lower in detection limit, the spongy platinum with the Pt purity being more than or equal to 99.995% can be detected, and the analysis efficiency and the accuracy of the detection result are greatly improved.
Drawings
FIG. 1 is a schematic diagram of a stamping die according to the present invention;
FIG. 2 is a schematic view of an embodiment of the bottom mold for sample unloading of the present invention;
labeled as: the upper die comprises a top die 10, a top die plate 11, a pressing part 12, a middle die 20, a middle die hole 21, a bottom die 30, a bottom die plate 31, a supporting part 32, a sample unloading bottom die 40, an upper stepped hole 41 and a lower stepped hole 42.
Detailed Description
The invention is further described below with reference to the figures and examples.
The method for testing the content of impurity elements in the sponge platinum comprises the following steps:
preparing sponge platinum to be tested into a sheet sample;
selecting a direct-reading spectrometer with an impurity element detection channel as a test instrument, selecting 6-8 standard samples with different impurity element contents, measuring the corresponding light intensity values of the impurity elements with different contents by using the direct-reading spectrometer, and implanting the standard curve of the impurity elements established by the direct-reading spectrometer into the direct-reading spectrometer; the different contents of the impurity elements mean that the contents of certain impurity elements in all standard samples are different, and the standard curve can be established in various ways, such as: for a certain impurity element, taking the light intensity value as a horizontal coordinate, taking the content of the impurity element as a vertical coordinate to establish a coordinate system, marking points representing each standard sample in the coordinate system, and connecting the points by using a smooth curve to form a standard curve; in the step, the selected direct-reading spectrometer is required to be ensured to be normally used, the direct-reading spectrometer is generally cleaned before being used so as to be in a clean state, then the light path of the direct-reading spectrometer is debugged, and finally the light intensity of the direct-reading spectrometer is corrected; the maximum content value of each impurity element in the standard sample is generally 100-200 ppm; before testing a standard sample, a method file table is generally required to be established, specifically, according to impurity elements to be measured, corresponding impurity element detection channels on a direct-reading spectrometer are determined, and information such as required drift correction samples is determined;
the way to ensure that a direct-reading spectrometer is usable is: turning on a power supply of the direct-reading spectrometer, stabilizing for a period of time, and judging whether parameters such as vacuum degree, detector temperature, instrument operation voltage, gas flow and the like are in a normal range;
the process of cleaning the direct-reading spectrometer generally comprises the following steps: thoroughly cleaning the inside and the outside of an instrument excitation system, detaching a sample carrying table, cleaning dust inside the sample carrying table and at an air outlet of the excitation system by using a dust collector, cleaning metal powder left after excitation on an electrode by using a metal brush, and wiping a quartz seat, a sealing ring, a tungsten carbide sheet and the like by using dust-free paper and a small amount of alcohol;
the process of debugging the direct-reading spectrometer generally comprises the following steps: testing a standard sample by a direct-reading spectrometer, wherein the standard sample contains impurity elements which are the same as those of the spongy platinum to be tested, and determining the optimal observation position according to the maximum intensity response value of each impurity element in the testing process;
the process of calibrating a direct-reading spectrometer generally comprises: determining a drift correction sample, performing a standardized test on the direct-reading spectrometer by using the calibration sample, and correcting the light intensity measured by the direct-reading spectrometer; the calibration sample is a Pt matrix sample standardized by the direct-reading spectrometer and is used for periodically correcting the test intensity value by the direct-reading spectrometer;
the direct-reading spectrometer implanted with the standard curve can automatically fit the standard curve and the linear correlation coefficient of each impurity element, and the direct-reading spectrometer can automatically convert the content value of each impurity element into a content value according to the response light intensity value during testing;
step three, measuring the known standard control sample with the content of each impurity element for more than 20 times by adopting a direct-reading spectrometer implanted with a standard curve to obtain the content of each impurity element, taking an average value as a test result, calculating the difference between the test result and a true value and the precision of the test result, if the difference between the test result and the true value and the precision of the test result are in an allowable range, indicating that the direct-reading spectrometer implanted with the standard curve is reliable, otherwise, repeating the step two and the step three; the standard control sample adopted in the step is used for confirming the accuracy of detection data, and a first type standard control sample with Pt purity of more than or equal to 99.99 percent and a second type standard control sample with Pt purity of more than or equal to 99.9 percent can be generally adopted; precision is a prerequisite to represent reproducibility of the measurement and to ensure accuracy;
step four, testing the sheet sample by using the direct-reading spectrometer verified to be reliable in step three, fixing the sheet sample on an excitation table of the direct-reading spectrometer, exciting 3-5 points on the test sheet sample, and averaging the results to obtain the content of each impurity in the sponge platinum; in this step, before testing the sheet sample, the excitation stage of the direct-reading spectrometer needs to be cleaned.
According to the method for testing the content of the impurity elements in the spongy platinum, after the spongy platinum to be tested is manufactured into a flaky sample, the flaky sample is directly tested by adopting a direct-reading spectrometer which is implanted with a standard curve of each impurity element and is verified to be reliable, various impurity elements such As Au, Ag, Pd, Rh, Ir, Ru, Al, As, B, Bi, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sb, Si, Sn, Ti, Zn, Zr and the like can be tested simultaneously, all impurities possibly brought in a spongy platinum purification process are basically covered, and the content of the impurities is far higher than 18 impurity elements required in national standards.
The spongy platinum is usually in the form of powder or particles, and in the step one, the granular spongy platinum is pressed into a sheet sample by using a stamping die. The stamping die has the function of gathering small sponge platinum particles together and pressing the small sponge platinum particles into a compact and flat sheet sample through external force. The stamping die may have various structures, and preferably, as shown in fig. 1, the stamping die includes a top die 10, a middle die 20, and a bottom die 30; the middle die 20 is provided with a middle die hole 21 penetrating through the middle die 20, the top die 10 comprises a top die plate 11 and a pressing part 12 arranged on the lower side of the top die plate 11 and matched with the middle die hole 21, and the bottom die 30 comprises a bottom die plate 31 and a supporting part 32 arranged on the upper side of the bottom die plate 31 and matched with the middle die hole 21. The sheet sample can be rapidly prepared by utilizing the stamping die, and impurities can be prevented from being brought in; in use, the middle mold 20 is mounted on the bottom mold 30, sponge platinum is filled in the middle mold hole 21, the top mold 10 is mounted on the middle mold 20, and appropriate pressure is applied to the top mold 10, so that a sheet-shaped sample can be prepared.
On the basis, in order to take out the sheet sample from the stamping die, as shown in fig. 2, the stamping die further includes a sample unloading bottom die 40, an upper stepped hole 41 adapted to the middle die 20 and a lower stepped hole 42 disposed in the sample unloading bottom die 40 and communicated with the upper stepped hole 41 are disposed at the top of the sample unloading bottom die 40, and the cross-sectional size of the lower stepped hole 42 is greater than that of the middle die hole 21. The upper stepped hole 41 and the lower stepped hole 42 are preferably coaxial circular holes, and the diameter of the upper stepped hole 41 is larger than that of the lower stepped hole 42.
Preferably, as shown in fig. 1 and 2, the process of making the sheet-like sample in step one is as follows:
a. cleaning each part of the stamping die by using dust-free paper dipped with alcohol for later use;
b. mounting the middle mold 20 on the bottom mold 30 such that the support portion 32 is inserted from the lower end of the middle mold hole 21; weighing 10-15 g of spongy platinum to be tested with the diameter of less than 3mm, and pouring the spongy platinum into a middle die hole 21; if the spongy platinum is too fluffy, when half of the spongy platinum is poured, the spongy platinum can be compacted by the top die 10 and then poured into the rest part;
c. mounting the top die 10 on the middle die 20 so that the pressing part 12 is inserted from the upper end of the middle die hole 21; then, pressing the top die 10 by using pressure equipment, controlling the pressure to be 25-35 Kpa, and continuously pressing for 15-20 s to obtain a sheet sample;
d. taking the middle die 20 containing the sheet sample and the top die 10 together from the bottom die 30, then mounting the middle die 20 on the sample unloading bottom die 40, and finally pressing the top die 10 to press the sheet sample into the lower step hole 42 and take out the sheet sample; when the top die is taken out, the pressure applied to the top die 10 needs to be controlled to be 10-20 KPa;
e. soaking the taken sheet sample in dilute hydrochloric acid for 5-10 min, then taking out and washing with clear water, then washing with absolute ethyl alcohol, and finally drying for later use.
As an effective scheme of the present invention, the method further includes, step three, measuring the high-purity sample by using a direct-reading spectrometer implanted with a standard curve for more than 10 times to obtain a test light intensity value of each impurity element, calculating a standard deviation σ of the light intensity value of each impurity element, and obtaining a detection lower limit of each impurity element according to a formula LOD ═ 3 σ × K; wherein, the Pt purity of the high-purity sample is more than 99.999 percent, K is the slope of the curve, the curve refers to the standard curve of the impurity element established in the step two, and K specifically refers to the slope of the point on the standard curve corresponding to the average value of the measured light intensity values of the impurity element. The high purity sample was used to determine the detection limit of the direct-reading spectrometer.
Specifically, in the third step, the lower detection limit of each impurity element is shown in the following table:
| impurity element | Au | Ag | Pd | Rh | Ir | Ru | Al | As | B | Bi |
| Lower detection limit (ppm) | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 1-2 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 |
| Impurity element | Ca | Cd | Co | Cr | Cu | Fe | Mg | Mn | Mo | Ni |
| Lower detection limit (ppm) | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 | 0.5-1 |
| Impurity element | Pb | Sb | Si | Sn | Ti | Zn | Zr | |||
| Lower detection limit (ppm) | 0.5-1 | 1-2 | 0.5-1 | 1-2 | 0.5-1 | 0.5-1 | 0.5-1 |
。
Therefore, the detection limit of the method for testing the content of the impurity elements in the spongy platinum is as low as 0.5ppm, and the detection limit of most impurity elements is below 1ppm and far superior to the detection limit of 5ppm of a plasma emission spectrometry. Therefore, the method can test the spongy platinum with the Pt purity of 99.90-99.99% to meet the national standard requirement, and can also test the spongy platinum with higher Pt purity.
Examples
The impurity content of sponge platinum with Pt purity of more than 99.99 percent is measured at a certain time, and the process is as follows:
s1, pressing the granular sponge platinum into a sheet sample by adopting a stamping die;
the stamping die comprises a top die 10, a middle die 20, a bottom die 30 and a sample unloading bottom die 40; the middle die 20 is provided with a middle die hole 21 for penetrating the middle die, the top die 10 comprises a top die plate 11 and a pressing part 12 which is arranged at the lower side of the top die plate 11 and is matched with the middle die hole 21, and the bottom die 30 comprises a bottom die plate 31 and a supporting part 32 which is arranged at the upper side of the bottom die plate 31 and is matched with the middle die hole 21; the top of the unloading bottom die 40 is provided with an upper step hole 41 matched with the middle die 20 and a lower step hole 42 arranged in the unloading bottom die 40 and communicated with the upper step hole 41, and the cross section size of the lower step hole 42 is larger than that of the middle die hole 21;
the process of pressing the sheet samples was as follows:
a. wiping all parts of the stamping die clean by using dust-free paper dipped with alcohol for later use, and preventing impurities from being brought in;
b. mounting the middle mold 20 on the bottom mold 30 such that the support portion 32 is inserted from the lower end of the middle mold hole 21; weighing 14.5g of spongy platinum to be tested with the diameter of less than 3mm, and pouring the spongy platinum into a middle die hole 21;
c. mounting the top die 10 on the middle die 20 so that the pressing part 12 is inserted from the upper end of the middle die hole 21; then, a pressure device is used for pressurizing the top die 10, the pressure is controlled to be 30Kpa, and the pressure is continuously applied for 15s, so that a sheet sample can be prepared;
d. taking the middle die 20 containing the sheet sample and the top die 10 together from the bottom die 30, then mounting the middle die 20 on the sample unloading bottom die 40, and finally pressing the top die 10 to press the sheet sample into the lower step hole 42 and take out the sheet sample; when taking out, applying pressure to the top die 10 to be controlled at 10 KPa;
e. soaking the taken out flaky sample in dilute hydrochloric acid for 8min, taking out the flaky sample, washing the flaky sample with clear water, washing the flaky sample with absolute ethyl alcohol, and finally drying the flaky sample for later use;
s2, selecting a direct-reading spectrometer with an impurity element detection channel as a test instrument, selecting 8 standard samples with different impurity element contents, measuring the corresponding light intensity values of the impurity elements with different contents by using the direct-reading spectrometer, and implanting the established standard curve of the impurity elements into the direct-reading spectrometer;
s3, measuring the standard control sample with known impurity element content for more than 20 times by using a direct-reading spectrometer (Spark-OES) implanted with a standard curve to obtain the impurity element content, taking an average value as a test result, calculating the difference between the test result and a true value and the precision of the test result, if the difference between the test result and the true value and the precision of the test result are within an allowable range, indicating that the direct-reading spectrometer implanted with the standard curve is reliable, otherwise, repeating the step two and the step three;
s4, testing the sheet sample by adopting the direct-reading spectrometer verified to be reliable in the third step, fixing the sheet sample on an excitation table of the direct-reading spectrometer, exciting 5 points of the tested sheet sample, and averaging the results to obtain the content of the impurities in the sponge platinum.
Comparative example
Weighing 14.5g of spongy platinum identical to the example, dissolving the spongy platinum with aqua regia, and testing the spongy platinum with a plasma emission spectrometer (ICP-OES); the test results were compared to the examples to verify the consistency of the test results, as shown in the table below.
Comparative and example test results comparative table:
according to the table, the detection limit of the test method provided by the invention to various impurity elements is as low as 0.5ppm, and the detection limit to most impurity elements is below 1ppm, which is far superior to the detection limit (5ppm) of the existing plasma emission spectrometry; while the content of impurity elements such as Rh, Ir and Ru is more than 5ppm, the difference between the detection result of the embodiment and the detection result of the comparative example is not large, so that the consistency of the test method provided by the invention and the test result of the existing test method is better.
Claims (9)
1. The method for testing the content of impurity elements in the spongy platinum is characterized by comprising the following steps:
preparing sponge platinum to be tested into a sheet sample;
selecting a direct-reading spectrometer with an impurity element detection channel as a test instrument, selecting 6-8 standard samples with different impurity element contents, measuring the corresponding light intensity values of the impurity elements with different contents by using the direct-reading spectrometer, and implanting the standard curve of the impurity elements established by the direct-reading spectrometer into the direct-reading spectrometer;
step three, measuring the known standard control sample with the content of each impurity element for more than 20 times by adopting a direct-reading spectrometer implanted with a standard curve to obtain the content of each impurity element, taking an average value as a test result, calculating the difference between the test result and a true value and the precision of the test result, if the difference between the test result and the true value and the precision of the test result are in an allowable range, indicating that the direct-reading spectrometer implanted with the standard curve is reliable, otherwise, repeating the step two and the step three;
and step four, testing the sheet sample by using the direct-reading spectrometer verified to be reliable in step three, fixing the sheet sample on an excitation table of the direct-reading spectrometer, exciting 3-5 points on the test sheet sample, and averaging the results to obtain the content of each impurity in the sponge platinum.
2. The method for testing the content of impurity elements in spongy platinum as claimed in claim 1, wherein: in the first step, a stamping die is adopted to press the granular sponge platinum into a sheet sample.
3. The method for testing the content of impurity elements in spongy platinum as claimed in claim 2, wherein: the stamping die comprises a top die (10), a middle die (20) and a bottom die (30); the middle die (20) is provided with a middle die hole (21) penetrating through the middle die, the top die (10) comprises a top die plate (11) and a pressing part (12) arranged on the lower side of the top die plate (11) and matched with the middle die hole (21), and the bottom die (30) comprises a bottom die plate (31) and a supporting part (32) arranged on the upper side of the bottom die plate (31) and matched with the middle die hole (21).
4. The method for testing the content of impurity elements in spongy platinum as claimed in claim 3, wherein: stamping die still including unloading a kind die block (40), the top of unloading a kind die block (40) is equipped with well mould (20) looks adaptation go up step hole (41) and set up in unloading a kind die block (40) and with last step hole (41) communicating lower step hole (42), the cross sectional dimension of lower step hole (42) is greater than the cross sectional dimension of well die hole (21).
5. The method for testing the content of impurity elements in spongy platinum as claimed in claim 4, wherein: the process of making the sheet sample in step one is as follows:
a. cleaning each part of the stamping die by using dust-free paper dipped with alcohol for later use;
b. mounting a middle die (20) on a bottom die (30) and embedding a supporting part (32) from the lower end of a middle die hole (21); weighing 10-15 g of spongy platinum to be tested with the diameter of less than 3mm, and pouring the spongy platinum into a middle die hole (21);
c. mounting a top die (10) on a middle die (20) to enable a pressing part (12) to be embedded into the upper end of a middle die hole (21); then, pressing the top die (10) by using pressure equipment, controlling the pressure to be 25-35 Kpa, and continuously pressing for 15-20 s to obtain a sheet sample;
d. taking the middle die (20) containing the sheet sample and the top die (10) from the bottom die (30), then mounting the middle die (20) on the sample unloading bottom die (40), and finally pressing the top die (10) to press the sheet sample into the lower step hole (42) and take out;
e. soaking the taken sheet sample in dilute hydrochloric acid for 5-10 min, then taking out and washing with clear water, then washing with absolute ethyl alcohol, and finally drying for later use.
6. The method for testing the content of impurity elements in spongy platinum as claimed in any one of claims 1 to 5, wherein: the impurity element includes at least one of Au, Ag, Pd, Rh, Ir, Ru, Al, As, B, Bi, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sb, Si, Sn, Ti, Zn and Zr.
7. The method for testing the content of impurity elements in spongy platinum as claimed in claim 6, wherein: the standard control samples comprise a first type of standard control sample with Pt purity more than or equal to 99.99% and a second type of standard control sample with Pt purity more than or equal to 99.9%.
8. The method for testing the content of impurity elements in spongy platinum as claimed in claim 6, wherein: step three, measuring the high-purity sample for more than 10 times by using a direct-reading spectrometer implanted with a standard curve to obtain a test light intensity value of each impurity element, calculating the standard deviation sigma of the light intensity value of each impurity element, and obtaining the detection lower limit of each impurity element according to the formula LOD (LoD-3 sigma K); wherein, the Pt purity of the high-purity sample is more than 99.999 percent, and K is the slope of the curve.
9. The method for testing the content of impurity elements in spongy platinum as claimed in claim 8, wherein: in the third step, the lower detection limit of each impurity element is shown in the following table:
。
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