CN101718720B - Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry - Google Patents
Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry Download PDFInfo
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Abstract
The invention relates to a method for detecting the content of carborundum impurities by applying an X-ray fluorescent spectrometry, comprising the following steps of: firstly, preparing a test sample wafer; secondly, preparing a standard sample wafer: (1) purifying a sample of carborundum; (2) purifying the carborundum to prepare puried carborundum; and (3) artificially preparing a standard sample and finally pressing the standard sample into a standard carborundum sample wafer; thirdly, establishing a working curve of the X-ray fluorescent spectrometry by the standard sample wafer; and fourthly, placing the prepared test sample wafer in an X-ray fluorescent spectrograph, measuring the sample wafer by the established working curve and automatically calculating the contents of various elements in the sample. By adopting the method, the workload for preparing standard series can be greatly reduced and the accuracy and the speed for preparation can be improved, thereby avoiding the defects of the traditional method for detecting the carborundum. The method is concise and rapid, meets the requirement of trade development, has great generalization and application values, and can be widely suitable for testing various samples by the X-ray fluorescent spectrum.
Description
Technical field
The present invention relates to the detection method of silit, particularly a kind of method that is applicable to R﹠D institution, universities and colleges, inspection center and corresponding manufacturer detecting content of carborundum impurities by applying X-ray fluorescent spectrometry.
Background technology
The X-ray fluorescence spectra analytic approach is a kind of modern universaling analysis method that various materials is carried out ultimate analysis, be widely used in departments such as environmental protection, geology, metallurgy, cement, inspection and quarantine, have characteristics such as precision height, measuring speed are fast, favorable reproducibility.The applying X-ray fluorescence spectrophotometer mainly is to carry out quantitative test, and the print for preparing by measurement draws each constituent content result in the sample.The preparation of print is mainly two kinds of the method sample preparation of melten glass sheet and compressing tablets, and the quality of print preparation directly has influence on the accuracy of measurement result.Characteristics such as the pressed disc method sample preparation has fast, makes things convenient for are widely used in the preparation of sample.
The foundation of x ray fluorescence spectrometry measurement curve needs the standard model of some, and the kind and the content range of element to be measured had certain requirement.As the standard model lazy weight, then need manually to prepare standard model, the way of conventional preparation standard model is the pure-oxide that takes by weighing element to be measured in the calculating ratio respectively, with claim various pure-oxide mixings, set up a standard model of working curve as x-ray fluorescence spectrometry, adopt what points to set up working curve, will prepare what corresponding standard samples.But the quod vide task is heavy, and requires various oxides accurately to take by weighing, to guarantee the quality of working curve.Because x-ray fluorescence spectrometry requires standard model to have identical matrix with testing sample, so can not only use pure-oxide, should add various oxides on matrix to be measured, could guarantee precision of test result.More as element to be measured, just require to prepare the standard model of a greater number.And some constituent content in each standard model is lower, in requisition for the only tens of milligrams of the pure-oxide quantity that adds, weighing equipment, environment, personnel, operation has all been proposed very high request.This shows, adopt traditional artificial preparation standard model method to be not easy to solve such problem.
The subject matter that the detection of silit runs into is:
1, the detection of silit requires to be generally silit, di-iron trioxide, alundum (Al, calcium oxide, magnesium oxide, phosphorus, sulphur equal size, but all be to adopt chemical analysis method, various compositions are tested separately, fail to reach various fast and effectively compositions and detect requirement simultaneously, can not satisfy the requirement that some users detect chromium, titanium etc. simultaneously.
2, lack the silit standard model
3, silicon carbide sample hardness height, the specimen preparation difficulty.
Summary of the invention
At above-mentioned these problems, the present invention proposes the method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry.By with various elements to be measured and flux fusion mixing, grind as the work matrix, join preparation standard sample in the silicon carbide sample after the purification more to scale, compressing tablet sample preparation then, the standard sample of photo that the configuration impurity content has certain gradient is started the new method that X-ray fluorescence spectra is manually prepared standard model, has realized the breakthrough of artificial preparation standard model mode, alleviate the workload of preparation standard series greatly, improved the accuracy and the speed of preparation.
Silit is China's traditional products as a kind of raw materials for production, is widely used in fields such as abrasive material, metallurgy, fire resistive material.Detection at silit, China has worked out the coherent detection standard respectively by its purposes, but all is to adopt chemical analysis method, and various compositions are tested separately, fail to reach various fast and effectively compositions and detect requirement simultaneously, and the chromium that proposes of some users, titanium etc. do not have detection method.At this situation, we have proposed to adopt x-ray fluorescence spectrometry to measure the imagination of multiple element in the silit simultaneously.But it applies in the detection of silicon carbide sample several difficult points are arranged still: at first lack the silit standard model.X-ray fluorescence spectrometry is higher to the degree of dependence of standard model, does not have good standard model just to be difficult to carry out testing accurately.Next silicon carbide sample hardness height, the specimen preparation difficulty.In development process, emphasis solves the preparation and the specimen preparation problem of serial silit standard model, to reach the X-ray fluorescence spectra test request.Overcome and in the preparation of silit standard model, related to silit purification and two difficult problems of impurity element adding method again.
A kind of method of detecting content of carborundum impurities by applying X-ray fluorescent spectrometry is characterized in that, comprises the steps:
(1), the preparation of test sample
Take by weighing a certain amount of silicon carbide sample, grind, take by weighing the sample of porphyrize then, add cementing agent, in mortar, grind well, more than pressurize 10s under 20～40T pressure, be pressed into test sample according to 5: 1～1: 1 ratio;
(2), the preparation of standard sample of photo
1. the purify sample preparation of silit
Take by weighing abrasive material level silit, adopt the ball-grinding machine of tungsten carbide material to grind more than 6 minutes;
2. silit is purified
Volatile matter in i, the removal silit
Take by weighing a certain amount of ground silicon carbide sample and place the platinum ware, put into more than 800 ℃ of muffle furnace calcination 1h, take out cooling;
Impurity silicon in ii, the removal silit
Drip the wetting silicon carbide sample of pure water with dropper, weight places to heat to the greatest extent on the electric furnace and does in 1: 2 ratio adding hydrofluorite, several nitric acid per sample, takes off cooling; Weight adds sulfuric acid in 1: 2 ratio adding hydrofluorite, 10: 1 ratio adding nitric acid, 100: 1 ratio per sample again, and electric furnace is heated to white cigarette and emits to the greatest extent, takes out and cools off;
Other impurity in iii, the removal silit
According to the ratio adding potassium pyrosulfate of silicon carbide sample weight in 1: 1, electric furnace is dried, and puts into muffle furnace and is warmed up to 420 ℃, more than the insulation 10min, continues to be warming up to 800 ℃, and fusion 10min takes out above back and cools off; The beaker of putting into a certain amount of 1: 1 hydrochloric acid boils, and silicon carbide sample is leached separate with the platinum ware; With the silicon carbide sample filtered while hot, with 1: 20 hydrochloric acid flushing of heat, be washed till no chlorion with pure water again till; The silicon carbide sample of cleaning is put into the platinum ware place on the electric furnace and dry, more than 800 ℃ of calcination 1h, take out cooling again; Repeating step iii promptly prepares pure product silit again, puts into exsiccator and preserves;
3. the artificial preparation of silit standard model
I, at first make the work matrix that contains various elements to be measured, being prepared as follows of work matrix: in the platinum yellow crucible, take by weighing a certain amount of primary standard substance after heating, drying is handled respectively, weight according to primary standard substance takes by weighing flux and remover by a certain percentage again, mixing, fusion in 1000～1125 ℃ of muffle furnaces, after the cooling, be poured into pulverize in the bowl mill of tungsten carbide alms bowl body stand-by;
Ii, the pure product silit that 2. is prepared into set by step that takes by weighing different proportion and work matrix, abundant mixing is prepared into the serial silit standard model that each detection elements content has certain gradient from low to high in bowl mill; Take by weighing the silit standard model that ground then and be pressed into the silit standard sample of photo according to step (1).
(3), set up x ray fluorescence spectrometry working curve
The silit standard sample of photo that is prepared into step (2) is set up the working curve of x ray fluorescence spectrometry;
(4), the measurement of sample
The test sample that step (1) is prepared into is put into the x ray fluorescence spectrometer, and the working curve that applying step (3) is set up is measured print, after the x ray fluorescence spectrometer detects, and the content of each element in the automatic calculation sample.
The beneficial effect that the present invention produced is: adopt this method, alleviated the workload of preparation standard series greatly, improved the accuracy and the speed of preparation, thereby avoided the existing deficiency of employing traditional technique in measuring silit.This method is succinct, quick, meets the requirement of Trade Development.Silicon carbide sample is purified and the mode of artificial preparation standard items has great popularizing value, can be widely used in X-ray fluorescence spectra and test in the various samples.
Below to selecting silit horizontal checkout sample, the mode that adopts traditional chemical analysis method and this method result to compare respectively.Chemical analysis results is finished by non-ferrous metal North China geological and mineral test center.The specimen chemical analysis results of six levels sees Table 1.Table 1 silit horizontal sample chemical analysis results
| Sample number into spectrum | SiC％ | Fe 2O 3 ％ | Al 2O 3 ％ | Cr 2O 3％ | TiO 2％ | MnO ％ | CaO％ | MgO ％ | P％ |
| 50％ | 51.43 | 2.08 | 5.64 | 0.025 | 0.21 | 0.052 | 0.37 | 0.18 | 0.026 |
| 60％ | 65.35 | 1.72 | 4.24 | 0.016 | 0.17 | 0.034 | 0.39 | 0.12 | 0.014 |
| 70％ | 79.67 | 1.32 | 2.81 | 0.0080 | 0.12 | 0.016 | 0.47 | 0.084 | 0.012 |
| 80％ | 86.83 | 1.14 | 1.94 | 0.0029 | 0.12 | 0.0077 | 0.50 | 0.073 | 0.0072 |
| 90％ | 90.98 | 0.88 | 1.50 | 0.0029 | 0.27 | 0.062 | 0.15 | 0.028 | 0.0047 |
| 97％ | 97.52 | 0.42 | 0.16 | 0.0016 | 0.030 | 0.033 | 0.022 | 0.0073 | 0.0006 |
Adopt this method to be prepared into print to six horizontal silicon carbide sample, see Table 2 with SRS3000 type Xray fluorescence spectrometer test result
This problem of table 2 silit horizontal sample methods analyst result
| Sample number into spectrum | ?SiC?％ | Fe 2O 3 ％ | A1 2O 3 ％ | Cr 2O 3 ％ | TiO 2％ | MnO％ | CaO％ | MgO％ | P％ |
| 50％ | 2.672 | 6.071 | 0.026 | 0.247 | 0.070 | 1.544 | 0.179 | 0.036 | |
| 60％ | 1.924 | 4.711 | Do not detect | 0.184 | 0.043 | 1.235 | 0.12 | 0.015 | |
| 70％ | 1.428 | 3.221 | Do not detect | 0.132 | 0.018 | 1.188 | 0.094 | 0.015 | |
| 80％ | 1.034 | 2.296 | Do not detect | 0.115 | 0.009 | 1.12 | 0.061 | 0.010 | |
| 90％ | 0.771 | 2.001 | Do not detect | 0.263 | 0.048 | 0.275 | Do not detect | 0.008 | |
| 97％ | 0.378 | 0.072 | Do not detect | 0.030 | 0.056 | 0.030 | Do not detect | 0.005 |
To 6 horizontal samples, adopt sample preparation methods provided by the invention and test condition, verify that by units such as The Second Institute of Oceanograghy,SOA, Ningbo Entry-Exit Inspection and Quarantine Bureau, Spanish mackerel circle Entry-Exit Inspection and Quarantine Bureau the result gathers and sees Table 3.
Table 3 horizontal sample proof list
In order to investigate this method and whether traditional chemical analytical approach test result exists systemic difference, both analysis results are compared analysis, see Table 4.
Table 4 silicon carbide sample chemical analysis results and XRF be compare of analysis as a result
Annotate: wherein the XRF measurement result adopts four unit testing results' such as Tianjin Entry-Exit Inspection and Quarantine Bureau, The Second Institute of Oceanograghy,SOA, Ningbo Entry-Exit Inspection and Quarantine Bureau, Spanish mackerel circle Entry-Exit Inspection and Quarantine Bureau mean value.
By two kinds of analytical approachs of each element being carried out the t check, confirm that there is not system deviation in both.
X-ray fluorescence spectrometry have detect fast, sample preparation multielement simultaneous determination, characteristics such as specimen preparation is simple, sensing range is wide, can be widely used in the detection of mineral products, metallurgic product, wherein the preparation of sample is problem that at first will solve and the accuracy that directly has influence on final detection result.The quantity of standard model, the characteristic of each element kind, content range and commodity itself has all restricted the application of x ray fluorescence spectrometry.
Embodiment
The invention will be further described below in conjunction with embodiment.
The method of detecting content of carborundum impurities by applying X-ray fluorescent spectrometry comprises the steps:
(1), the preparation of test sample
Take by weighing a certain amount of silicon carbide sample, grind, take by weighing the sample of porphyrize then, add cementing agent (wax powder) according to 5: 1 ratios, grind well in mortar, pressurize 20～40s is pressed into test sample under 20～40T pressure.
By experimental study to sample preparation material, milling apparatus, time, the preparation method who determines silicon carbide sample is: take by weighing a certain amount of approximately silicon carbide sample, adopt the ball-grinding machine of tungsten carbide material to grind several minutes, with reach test result stable, pollute controlled, fineness enough, the requirement little to loss in head.
(2), the preparation of standard sample of photo
1. the purify sample preparation of silit
Take by weighing 120# abrasive material level silit, adopt the ball-grinding machine of tungsten carbide material to grind 6 minutes;
2. silit is purified
Volatile matter in i, the removal silit
Take by weighing a certain amount of ground silicon carbide sample and place the platinum ware, put into 800 ℃ of muffle furnace calcination 1.5h, remove volatile matter, take out cooling;
Impurity silicon in ii, the removal silit
Drip the wetting silicon carbide sample of pure water with dropper, weight places to heat to the greatest extent on the electric furnace and does in 1: 2 ratio adding hydrofluorite, several nitric acid per sample, takes off cooling; Weight adds sulfuric acid in 1: 2 ratio adding hydrofluorite, 10: 1 ratio adding nitric acid, 100: 1 ratio per sample again, and electric furnace is heated to white cigarette and emits to the greatest extent, takes out and cools off;
Other impurity in iii, the removal silit
According to the ratio adding potassium pyrosulfate of silicon carbide sample weight in 1: 1, electric furnace is dried, and puts into muffle furnace and is warmed up to 420 ℃, and insulation 10min continues to be warming up to 800 ℃, takes out cooling behind the fusion 10min; Put into a certain amount of 1: 1 hydrochloric acid (volume with hydrochloric acid did not have the platinum ware to be as the criterion) beaker boil, silicon carbide sample is leached separates with the platinum ware; With the silicon carbide sample filtered while hot, with 1: 20 hydrochloric acid flushing of heat, be washed till no chlorion with pure water again till; The silicon carbide sample of cleaning is put into the platinum ware place on the electric furnace and dry,, take out cooling again in 800 ℃ of calcination 1h; Repeating step iii promptly prepares pure product silit again, puts into exsiccator and preserves.
Do not contain other impurity by chemical method purification silit to guarantee it, through removing volatile matter, just can be met the extremely pure silit of requirement of experiment after hydrofluorite silica removal repeatedly, the potassium pyrosulfate removal of impurity like this.
3. the artificial preparation of silit standard model
At first make the work matrix that contains various elements to be measured, to 2. going into the work matrix by different proportion Erbium-doped in the silit parent of preparation set by step, be mixed with the serial silit standard items of required combination in any again.The standard film of preparation is used to set up the working curve of x ray fluorescence spectrometry.China does not also have commercially available silit standard model at present, can not get the pure product of silit yet.Therefore, need artificial preparation silit standard items, to satisfy the needs of instrumental analysis.This work relates to two difficult problems: how to obtain pure product silit and how in pure product silit, to add element to be measured, and even, reliable with the solid silit standard model that guarantees preparation.
I, at first make the work matrix that contains various elements to be measured, being prepared as follows of work matrix: in the platinum yellow crucible, take by weighing a certain amount of primary standard substance after heating, drying is handled respectively, weight according to primary standard substance takes by weighing flux and remover by a certain percentage again, mixing, fusion in 1000～1125 ℃ of muffle furnaces, after the cooling, be poured into pulverize in the bowl mill of tungsten carbide alms bowl body stand-by;
Ii, the pure product silit that 2. is prepared into set by step that takes by weighing different proportion and work matrix, abundant mixing is prepared into the serial silit standard model that each detection elements content has certain gradient from low to high in bowl mill; Take by weighing the silit standard model that ground then and be pressed into the silit standard sample of photo according to step (1).
(3), set up x ray fluorescence spectrometry working curve
The silit standard sample of photo that is prepared into step (2) is set up the working curve of x ray fluorescence spectrometry;
The measuring condition of the working curve of every element to be measured is set up voluntarily according to the requirement of the x ray fluorescence spectrometer of different manufacturers.
(4), the measurement of sample
The test sample that step (1) is prepared into is put into the x ray fluorescence spectrometer, and the working curve that applying step (3) is set up is measured print, after the x ray fluorescence spectrometer detects, and the content of each element in the automatic calculation sample.
Embodiment:
(1), the preparation of test sample
Take by weighing the 1.5g silicon carbide sample, adopt the ball-grinding machine of tungsten carbide material to grind 6 minutes, accurately take by weighing the sample 1.0g of porphyrize then, add 0.2g wax powder, grind well, pressurize 30s is pressed into test sample under 30T pressure.
(2), the preparation of standard sample of photo
1. the purify sample preparation of silit
Take by weighing 25.0000g high-grade 120# abrasive material level silit, adopt the ball-grinding machine of tungsten carbide material to grind 6 minutes.
2. silit is purified
Volatile matter in i, the removal silit
Take by weighing the ground silicon carbide sample of 20.0000g and place the platinum ware, put into 800 ℃ of muffle furnace calcination 1.5h, remove volatile matter, take out cooling.
Impurity silicon in ii, the removal silit
Drip the silicon carbide sample of the wetting i step of pure water with dropper, amount adds 40mL hydrofluorite, four (1: 1) nitric acid (1 part of pure water mixes with 1 part of nitric acid) per sample, places on the electric furnace heating most dried, takes off cooling.Add 40mL hydrofluorite, 2mL nitric acid, 0.2mL1 again: 1 sulfuric acid (1 part of pure water mixes with 1 part of sulfuric acid), electric furnace are heated to after white cigarette emits to the greatest extent, take out cooling.
Other impurity in iii, the removal silit
Add the 20g potassium pyrosulfate in ii step silicon carbide sample, electric furnace is dried, put into muffle furnace and begin to warm to 420 ℃, insulation 10min continues to be warming up to 800 ℃, take out cooling behind the fusion 10min, put into 80mL1: the 200mL beaker of 1 hydrochloric acid (1 part of pure water and 1 part of mixed in hydrochloric acid) boils, and silicon carbide sample is leached separate with the platinum ware, with the silicon carbide sample filtered while hot, with 1: 20 hydrochloric acid flushing of heat several times, again with pure washing 5～10 times till do not have a chlorion.The silicon carbide sample of cleaning is put into the platinum ware to be placed on the electric furnace and dries, again in 800 ℃ of calcination 1h, after taking out cooling, again repeating step iii (add again the 20g potassium pyrosulfate soak molten once, according to abovementioned steps clean, oven dry, calcination etc.), promptly prepare pure product silit, put into exsiccator and preserve.
3. the artificial preparation of silit standard model
I, at first make the work matrix that contains various elements to be measured, being prepared as follows of work matrix: in the platinum yellow crucible, take by weighing the primary standard substance Fe after heating, drying is handled respectively
2O
3And Al
2O
3Each 2.0000g, CaO, MgO, Cr
2O
3, MnO
2, TiO
2, KH
2PO
4Each 1.0000g, took by weighing flux again 12: 22 (lithium metaborate: 10.0000g lithium tetraborate), remover (ammonium iodide) 0.3000g, mixing, fusion is 20 minutes in 1000 ℃ of muffle furnaces, be poured into after the cooling pulverize in the bowl mill of tungsten carbide alms bowl body stand-by.
Ii, take by weighing pure product silit and work matrix that 2. different proportion be prepared into set by step, abundant mixing in bowl mill is prepared into the serial silit standard model that each detection elements content has certain gradient from low to high, claims the sample ratio to see Table 5.Take by weighing the silit standard model 1.0000g and the 0.2g wax powder mixing that ground then and grind well in mortar, pressurize was pressed into serial silit standard sample of photo in 30 seconds under 30 tons of pressure.Each detection elements content of serial silit standard items of preparation sees Table 6
The sample weighting amount of table 5, preparation silit standard model purification silit and work matrix
| The standard model numbering | Purification silit (g) | Work matrix (g) |
| 1 | 1.0000 | 0.0000 |
| 2 | 0.9800 | 0.0200 |
| 3 | 0.9600 | 0.0400 |
| 4 | 0.9400 | 0.0600 |
| 5 | 0.9200 | 0.0800 |
| 6 | 0.9000 | 0.1000 |
| 7 | 0.8000 | 0.2000 |
| 8 | 0.7000 | 0.3000 |
| 9 | 0.6000 | 0.4000 |
| 10 | 0.5000 | 0.5000 |
| 11 | 0.4000 | 0.6000 |
| 12 | 0.3000 | 0.7000 |
| 13 | 0.2000 | 0.8000 |
| 14 | 0.1000 | 0.9000 |
| 15 | 0.0000 | 1.0000 |
The silicon-carbide series standard items of the artificial preparation of table 6 contain scale
| The standard model numbering | SiC％ | Fe2O3％ | Al2O3％ | Cr2O3％ | TiO2％ | MnO2％ | CaO％ | MgO％ | P％ |
| 1 | 100.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00000 |
| 2 | 98.00 | 0.20 | 0.20 | 0.10 | 0.10 | 0.10 | 0.10 | 0.10 | 0.02276 |
| 3 | 96.00 | 0.40 | 0.40 | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 | 0.04552 |
| 4 | 94.00 | 0.60 | 0.60 | 0.30 | 0.30 | 0.30 | 0.30 | 0.30 | 0.06828 |
| 5 | 92.00 | 0.80 | 0.80 | 0.40 | 0.40 | 0.40 | 0.40 | 0.40 | 0.09104 |
| 6 | 90.00 | 1.00 | 1.00 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.11380 |
| 7 | 80.00 | 2.00 | 2.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 0.22760 |
| 8 | 70.00 | 3.00 | 3.00 | 1.50 | 1.50 | 1.50 | 1.50 | 1.50 | 0.34140 |
| 9 | 60.00 | 4.00 | 4.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 0.45520 |
| 10 | 50.00 | 5.00 | 5.00 | 2.50 | 2.50 | 2.50 | 2.50 | 2.50 | 0.56900 |
| 11 | 40.00 | 6.00 | 6.00 | 3.00 | 3.00 | 3.00 | 3.00 | 3.00 | 0.68280 |
| 12 | 30.00 | 7.00 | 7.00 | 3.50 | 3.50 | 3.50 | 3.50 | 3.50 | 0.79660 |
| 13 | 20.00 | 8.00 | 8.00 | 4.00 | 4.00 | 4.00 | 4.00 | 4.00 | 0.91040 |
| 14 | 10.00 | 9.00 | 9.00 | 4.50 | 4.50 | 4.50 | 4.50 | 4.50 | 1.02420 |
| 15 | 0.00 | 10.00 | 10.00 | 5.00 | 5.00 | 5.00 | 5.00 | 5.00 | 1.13800 |
(3), set up x ray fluorescence spectrometry working curve
The silit standard sample of photo that is prepared into step (2) is set up the working curve of x ray fluorescence spectrometry;
To the silit standard sample of photo that makes, adopt SRS3000 type Xray fluorescence spectrometer to measure, through selecting condition determination such as table 7:
Each detection elements measuring condition of table 7SRS3000 type Xray fluorescence spectrometer
| Element/spectral line | Electric current mA | Voltage Kv | 2θ℃ | Slit | Crystal | The background position |
| SiKα | 40 | 30 | 109.2 | 0.15 | PET | No |
| FeKα | 50 | 50 | 57.5 | 0.15 | LiF200 | No |
| AlKα | 100 | 30 | 145.09 | 0.46 | PET | 143.2 |
| CrKα | 50 | 60 | 69.59 | 0.46 | LiF200 | 74.4 |
| TiKα | 50 | 60 | 86.12 | 0.46 | LiF200 | No |
| MnKα | 50 | 60 | 62.96 | 0.46 | LiF200 | No |
| CaKα | 60 | 50 | 113.07 | 0.46 | LiF200 | 115.0 |
| MgKα | 100 | 30 | 20.70 | 0.46 | OVO55 | No |
| PKα | 100 | 30 | 89.4 | 0.46 | PET | No |
Series standard product with 2. step is prepared adopt above condition of work, set up working curve on the SRS3000X ray fluorescence spectrometer.The empirical coefficient method correction software of utilization Siemens Company exploitation is proofreaied and correct spectral line enhancing, absorption effect.
(4), the measurement of sample
The test sample that step (1) is prepared into is put into the x ray fluorescence spectrometer, and the working curve that applying step (3) is set up is measured print, after the x ray fluorescence spectrometer detects, and the content of each element in the automatic calculation sample.
By to the preparation method of silicon carbide sample lapping mode, method of purification, standard model and the research of test condition, clear and definite can adopt the X-ray fluorescence spectra method to measure multiple element in the silit simultaneously, have reappearance and repeatability preferably, method is succinct, quick, meets the requirement of Trade Development.
Silicon carbide sample of the present invention is purified and artificial preparation standard items mode has great popularizing value, can be widely used in X-ray fluorescence spectra and test in the various samples.
Claims (1)
1. the method for a detecting content of carborundum impurities by applying X-ray fluorescent spectrometry is characterized in that, comprises the steps:
(1), the preparation of test sample
Take by weighing a certain amount of silicon carbide sample, grind, take by weighing the sample of porphyrize then, add cementing agent with 5: 1～1: 1 part by weight, in mortar, grind well, under 20～40 tons of pressure, more than the pressurize 10s, be pressed into test sample according to sample and cementing agent;
(2), the preparation of standard sample of photo
1. the purify sample preparation of silit
Take by weighing abrasive material level silit, adopt the ball-grinding machine of tungsten carbide material to grind more than 6 minutes;
2. silit is purified
Volatile matter in i, the removal silit
Take by weighing a certain amount of ground silicon carbide sample and place the platinum ware, put into more than 800 ℃ of muffle furnace calcination 1h, take out cooling;
Impurity silicon in ii, the removal silit
Drip the wetting silicon carbide sample of pure water with dropper, weight per sample is 1: 2 ratio adding hydrofluorite according to the w/v of sample and hydrofluorite, the unit of wherein wt is g, and the unit of volume is ml, drips several nitric acid, place to heat to the greatest extent on the electric furnace and do, take off cooling; Weight per sample again, according to the w/v of sample and hydrofluorite is that 1: 2 ratio adds hydrofluorite, and the unit of wherein wt is g, and the unit of volume is ml, according to the w/v of sample and nitric acid is that 10: 1 ratio adds nitric acid, the unit of wherein wt is g, and the unit of volume is ml, is that 100: 1 ratio adds sulfuric acid according to the w/v of sample and sulfuric acid, the unit of wherein wt is g, the unit of volume is ml, and electric furnace is heated to white cigarette and emits to the greatest extent, takes out cooling;
Other impurity in iii, the removal silit
According to silicon carbide sample weight, add potassium pyrosulfate according to sample and potassium pyrosulfate with 1: 1 part by weight, electric furnace is dried, and puts into muffle furnace and is warmed up to 420 ℃, more than the insulation 10min, continues to be warming up to 800 ℃, and fusion 10min takes out cooling in above back; The beaker of putting into certain water gaging and hydrochloric acid volume ratio and be 1: 1 hydrochloric acid solution boils, and silicon carbide sample is leached separate with the platinum ware; With the silicon carbide sample filtered while hot, according to sample and the hydrochloric acid w/v with 1: 20, the unit of wherein wt is g, and the unit of volume is ml, with the hydrochloric acid flushing of heat, be washed till no chlorion with pure water again till; The silicon carbide sample of cleaning is put into the platinum ware place on the electric furnace and dry, more than 800 ℃ of calcination 1h, take out cooling again; Repeating step iii promptly prepares pure product silit again, puts into exsiccator and preserves;
3. the artificial preparation of silit standard model
I, at first make the work matrix that contains various elements to be measured, being prepared as follows of work matrix: in the platinum yellow crucible, take by weighing a certain amount of primary standard substance after heating, drying is handled respectively, weight according to primary standard substance takes by weighing flux and remover by a certain percentage again, mixing, fusion in 1000～1125 ℃ of muffle furnaces, after the cooling, be poured into pulverize in the bowl mill of tungsten carbide alms bowl body stand-by;
Ii, the pure product silit that 2. is prepared into set by step that takes by weighing different proportion and work matrix, abundant mixing is prepared into the serial silit standard model that each detection elements content has certain gradient from low to high in bowl mill; Take by weighing the silit standard model that ground then and be pressed into the silit standard sample of photo according to step (1);
(3), set up x ray fluorescence spectrometry working curve
The silit standard sample of photo that is prepared into step (2) is set up the working curve of x ray fluorescence spectrometry;
(4), the measurement of sample
The test sample that step (1) is prepared into is put into the x ray fluorescence spectrometer, and the working curve that applying step (3) is set up is measured print, after the x ray fluorescence spectrometer detects, and the content of each element in the automatic calculation sample.
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