36 results about "Glow Discharge Mass Spectrometry" patented technology

The invention relates to a determination method for trace impurities in a rare metal, particularly to a determination method for trace impurities in high purity indium. The determination method comprises: (1) cutting a sample into a sheet, washing oil stain on the sample surface with toluene, washing with ultrapure water, etching for 8 min with 50% (volume concentration) nitric acid, repeatedly rinsing with ultrapure water, storing in methanol, and taking and drying under an infrared lamp before analysis; (2) placing the sample in a sample clamper, pushing into an ion source chamber, respectively adjusting the discharge voltage and the discharge current to 0.9-1.2 kV and 40-45 mA when the vacuum degree achieves 2.2-2.4 mbar, and sputtering for about 30-40 min, wherein generally stabilization of signals of Na, Fe and Ca easily introducing contamination is adopted as the reference so as to eliminate possibly-produced contamination during the sample preparation process; and (3) respectively adjusting the discharge voltage and the discharge current to 0.9-1.2 kV and 40-45 mA, carrying out high voltage discharge, collecting the ion signals of the elements to be detected, and calculating the concentration of the impurity elements to be detected according to the quantitative analysis principle of the glow discharge mass spectrometer. The method has characteristics of simple operation, less interference and short process, and can well meet requirements of determination of trace impurities in high purity indium.

A direct current glow discharge mass-spectrography method for determination of impurity elements in high purity alpha-Al2O3 comprises the following steps: (1) evenly mixing Al2O3 powder and copper powder according to the proportion, then tabletting the mixed powder, blowing away the powder on the surface of the sample with N2, and filling the sample into a sample pool; (2) setting the flow of discharge gas at 500 mL / min, discharge current of 30 mA and ion source cooling temperature at 5-25 DEG C, and pre-sputtering for 15 min; (3) acquiring the signal intensity of the element to be measured under the experimental conditions set in step (2), defining the total sum of signal intensity generated by Al, O and Cu as 100%, and calculating the element content to be measured in the mixed powder according to the ratio of the signal intensity of the element to be measured to the total signal intensity of the three elements Al, O and Cu; and deducting the content of the element to be measured in the copper powder to obtain the content of the element to be measured in Al2O3. The invention realizes the determination of the content of impurity elements in non-conductive alpha-Al2O3 powder by the direct current glow discharge mass-spectrometry method, and the determination results are basically consistent with those of the DC arc emission spectroscopy method.

The invention provides a cage-like sampling device for glow discharge mass spectrometry and a sample test method, and aims at solving the difficulty of the glow discharge mass spectrometry (GD-MS) foranalyzing different types of samples with different sizes. The cage-like sampling device comprises a cage-like metal groove and a metal handle which is arranged at one end of the cage-like metal groove; the metal handle is used for fixing the cage-like sampling device relative to a glow discharge mass spectrometer; a sample loading port is formed in the other end of the cage-like metal groove toload and unload samples; the cage-like metal groove is prepared by carrying out punching and machining on a metal sheet with the purity greater than 99.995%; the size of the cage-like metal groove issmaller than the size of a glow discharge battery of the glow discharge mass spectrometer and the cage-like metal groove can be put in the glow discharge battery; and the volume of the cage-like metalgroove is smaller than the volume of the glow discharge battery.

One or more embodiments of the invention provide a glow discharge mass spectrometry high-purity gallium testing method, which comprises the following steps: heating solid gallium to obtain liquid gallium, cleaning a polytetrafluoroethylene mold, air-drying, putting the polytetrafluoroethylene mold on a cooling device, pouring the liquid gallium into the polytetrafluoroethylene mold placed on the cooling device, transferring the polytetrafluoroethylene mold into an ultra-clean bench within a set time, standing until a formed sample is obtained, fixing the formed sample, charging the sample into a GDMS sample chamber, vacuumizing, cooling the sample in a semiconductor refrigeration mode, discharging within the set time, and removing surface pollution through discharge sputtering; after the signal is stable, collecting and analyzing data are through the GDMS, and after the analysis is finished, recording and storing the data, so that the purpose that the plane to be measured can be obtained through a form conversion mode for low-melting-point metal such as gallium and indium for measurement is achieved.

The invention relates to a method for preparing a high-pure-cobalt solution through stirring and extraction, and belongs to the technical field of preparing a metal material. The method comprises: preparing a cobalt solution in a high-level extraction tank; adding sulfonated kerosene, a P507 extractant, and sodium hydroxide in a low-level extraction tank, performing stirring for saponification, and pumping the obtained product into the high-level extraction tank for stirring and extraction to enable cobalt in the cobalt solution extracted into an organic phase; adding hydrochloric acid to wash the loading organic phase while performing stirring, and performing back extraction to prepared a cobalt-rich liquid; adding a macroporous adsorption resin for deep purification, and performing condensation and electrolytic deposition; and performing vacuum melting of electrolytic deposited cobalt to obtain a high-pure cobalt ingot. The purity of the high-pure cobalt ingot is analyzed by glow discharge mass spectrometry, and the purity of more than 70 kinds of elements in the cobalt ingot is more than 99.999%. According to the invention, high selectivity of liquid-liquid extraction and properties, such as turbulence and shear force, of stirring are combined to enhance the reaction process and to improve the purification capability of the cobalt solution. The method is simple, and is easy to operate and low in cost. Processes in the method are relatively independent, so that the method is high in flexibility. Chemical materials are less in consumption, and the equipment is high in productivity, so that the method benefits scale production.

The invention relates to a method of measuring the thickness of an Nd-Fe-B alloy coating, which belongs to the technical field of coating detection. Absolute ethanol is used for cleaning the surface of the Nd-Fe-B alloy coating, and a nitrogen gas is used for drying; glow discharge mass spectrometry (GD-MS) is adopted to carry out all-element qualitative measurement on the alloy coating, and the coating type is judged; the discharge current of a GD-MS instrument is adjusted to be 20 mA, the discharge gas Ar flow is 400 mL/min, and corresponding lens parameters are adopted for each coating; uninterrupted sputtering is carried out on the alloy coating, data are collected for one time at each 15 seconds until a Fe element content rises straightly, and sputtering is stopped; the obtained data are used for drawing an element mass fraction-sputtering time distribution map, a boundary point in each layer is found out on the map, and the sputtering time in each coating layer is obtained; and according to the sputtering rate and the sputtering time of each layer, the thickness of each coating is calculated, the method is simple and easy to operate, and the accuracy is high.

The invention provides a sample preparation method of molybdenum scraps in glow discharge mass spectrometry, which comprises the following steps of: placing molybdenum scraps to be detected in a blind hole of a conductive substrate, and then tabletting to complete sample preparation of the molybdenum scraps. According to the invention, a blind hole is formed in a conductive substrate, and molybdenum chips are subjected to sample preparation by using the blind hole of the conductive substrate, so that the pollution possibly caused by the sample is reduced, and the accuracy of detection data is improved; and the sample preparation success rate of the sample preparation method can reach 95% or above.

The invention provides a sample preparation method and a test method of glow discharge mass spectrometry ammonium paratungstate powder. The method comprises the steps: forming a groove in the surface of a high-purity indium sheet, cleaning the indium sheet, transferring the ammonium paratungstate powder into the groove by using a cleaned medicine spoon, and compacting by using a press machine to obtain a sample to be tested. According to the sample preparation method, introduction of impurities can be fully avoided, the analysis time is shortened, and the accuracy of a test result is improved; and the test signal obtained by the test method is strong, and the sensitivity is high.

The invention relates to a method for analyzing small-size conductive and non-conductive materials by applying glow discharge mass spectrometry, and belongs to the field of material analysis. The method comprises the following steps: placing graphite powder in an aluminum cup, and slightly vibrating the aluminum cup to flatten the surface of the graphite powder; placing a small-size conductive material or a non-conductive material on the graphite powder; covering with a plurality of layers of parchment paper; pressing by using a tablet press to prepare a test sample; and carrying out direct current glow discharge mass spectrometry. According to the analysis method, grinding, sintering and heating are not needed, the pretreatment is simple, and the pollution is avoided; the problem that the metal element cannot be measured when the metal is used as a conducting medium and the mass spectrum interference formed by the metal element are avoided; the analysis time is shortened, and the analysis efficiency is improved; the method can be suitable for analysis of small-size conductive materials such as crumb-shaped, granular and powdery conductive materials and fine-granular and powdery non-conductive materials, and is high in universality and wide in application range; the method has good discharge stability, analysis repeatability and analysis accuracy.

The invention discloses a testing method for detecting a low-melting-point material by glow discharge mass spectrometry. The testing method comprises the following steps of 1, manufacturing a metal carrier; 2, obtaining a treated metal carrier; 3, a liquid low-melting-point material being obtained, and then a proper amount of the liquid low-melting-point material being taken and poured into the circular groove; 4, sequentially rinsing the surface of the solidified to-be-detected sample with deionized water ethanol for three times, and then naturally airing and putting into a sample cup; and 5, cooling the ion source chamber, connecting the sample cup with an electrode, pushing the sample cup into the ion source chamber, and detecting impurity components. According to the method, complex pretreatment is avoided, so analysis efficiency is improved, impurity interference caused by pretreatment is avoided for component analysis of the high-purity low-melting-point material, accuracy of an analysis result is ensured, and the method can be used for simultaneously analyzing multiple elements, has advantages of high analysis speed, small matrix effect, good environmental friendliness and the like, and has wide application prospects.