CN101303307B - Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide - Google Patents
Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide Download PDFInfo
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- CN101303307B CN101303307B CN200810031711XA CN200810031711A CN101303307B CN 101303307 B CN101303307 B CN 101303307B CN 200810031711X A CN200810031711X A CN 200810031711XA CN 200810031711 A CN200810031711 A CN 200810031711A CN 101303307 B CN101303307 B CN 101303307B
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Abstract
The invention discloses an analysis and detection method for impurity elements such as aluminum, calcium, ion, molybdenum, niobium, titanium, tungsten and the like in chromium carbide. The method comprises adding a chromium carbide sample into a dissolving cup, adding hydrofluoric acid, sulphuric acid and nitric acid sequentially, stirring, charging into a sealed high-pressure jar; putting the sealed high-pressure jar into a microwave extinguishing instrument for two times of microwave extinguishment; taking the high-pressure jar out of the microwave extinguishing instrument for cooling, transferring the dissolved chromium carbide liquid sample into a volumeric flask, diluting to a predetermined index, stirring; preparing a chromium substrate matched mixed standard solution series of aluminum, calcium, iron, molybdenum, niobium, titanium and tungsten; measuring element emission power of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten or the like in a blank liquid sample, a chromium carbide liquid sample and the prepared series mixed standard solution by an inductively coupled plasma atomic emission spectrometer in the same time, obtaining the analysis result by checking a standard working curve or by linear equation calculation. The invention adopts two times of microwave extinguishment using the mixed acid, solves the problem of hardness in chromium carbide decomposition, having a measurement range from 0.010% to 1.00%, which is high in accuracy, and good in precision.
Description
Technical field
The present invention relates to the analyzing detecting method of seven kinds of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the analyzing and testing of seven kinds of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten, particularly chromium carbide.
Background technology
In existing chromium carbide chemical analysis method, only main content chromium is measured, wherein impurity element there is not corresponding chemical analysis method.But when chromium carbide added in the alloy as the wimet adjuvant, the height of impurity content directly affected the performance of wimet in the chromium carbide.In order to guarantee the quality of hart metal product, must carry out analyzing and testing to seven kinds of impurity elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide, owing to need in the chromium carbide impurity element measured many and content is lower, should select for use the inductively coupled plasma atomic emission spectrometer with higher sensitivity to carry out assay determination, this is industry technician's a common recognition.Yet, chromium carbide is an insoluble compound, be difficult to decompose fully, though can decompose with the potassium pyrosulfate fusion method, or with the dissolving of a large amount of mixture of sulfuric phosphoric acid, but may there be the problem of introducing a large amount of impurity elements in the skip test liquid of above-mentioned molten (molten) agent, is not suitable for inductively coupled plasma atomic emission spectrometer and measures, and also is unfavorable for guaranteeing the accuracy to impurities analysis mensuration in the chromium carbide.Therefore, chromium carbide can be decomposed fully, artificially do not introduce a large amount of impurity elements again, become and adopt inductively coupled plasma atomic emission spectrometer to measure seven kinds of one technical barriers that impurity element must solve such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide.
Summary of the invention
Purpose of the present invention just is to solve above-mentioned chromium carbide and is difficult to decompose technical barrier completely, provide a kind of inductively coupled plasma atomic emission spectrometer that is applicable to measure, artificially do not introduce the foreign impurity element again, measure the analyzing detecting method of seven kinds of impurity elements such as aluminium in the chromium carbide, calcium, iron, molybdenum, niobium, titanium, tungsten exactly, fill up the blank of impurities analysis detection method in the chromium carbide that exists in the prior art.
For realizing that the object of the invention has adopted a kind of Microwave Digestion to decompose the chromium carbide sample, select for use hydrofluorite, sulfuric acid, nitric acid acid mixture to make solvent, in pressure pan, the chromium carbide sample is carried out micro-wave digestion twice; Adopt chromium matrix coupling hybrid standard curve simultaneously, on inductively coupled plasma atomic emission spectrometer, directly measure impurity elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten.
Adopting acid mixture to carry out micro-wave digestion decomposition chromium carbide sample is that sample is placed closed container microwave energy heated sample, and microwave energy adds hot acid and test portion rapidly, and redox reaction and themopositive reaction take place, and produces gas.The gas that produces forms the high pressure atmosphere in the container, thereby has improved boiling point, oxidability and the activity of solvent, makes sample to clear up in very short time.Because by the best operating condition of optimizing, carry out micro-wave digestion once, still have a spot of chromium carbide test portion not dissolve, if pressure boost again, time expand, unfavorable to pressure pan, so after taking to treat the pressure pan cool to room temperature, carry out the micro-wave digestion second time again, the chromium carbide test portion is dissolved fully through twice micro-wave digestion.Concrete technical scheme comprises:
(1) the chromium carbide test portion is placed the molten sample cup of teflon, with behind the deionized water purge wall of cup, add hydrofluorite, sulfuric acid, nitric acid more successively earlier, mixing covers bowl cover, and molten sample cup is put into airtight pressure pan;
(2) pressure pan is placed microwave dissolver, the selected working pressure of mode and the digestion time that increase progressively stage by stage by working pressure carry out the micro-wave digestion first time continuously, after clearing up and finish the first time pressure pan is shifted out and cool to room temperature, and then place microwave dissolver to carry out the micro-wave digestion second time pressure pan by clearing up same condition of work with the first time.
(3) take out pressure pan from microwave dissolver, jar is opened in the cooling back in vent cabinet, and consoluet chromium carbide test solution is moved in 100mL (milliliter) the plastics volumetric flask, is diluted to scale with deionized water, mixing.
(4) aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of preparation chromium matrix coupling so just can be eliminated the matrix effect influence of chromium carbide test solution;
(5) under selected instrument condition of work, the mixed standard solution series of blank, chromium carbide test solution and preparation is measured the emissive porwer of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten simultaneously on inductively coupled plasma atomic emission spectrometer, find the mass concentration of corresponding tested element more according to a conventional method from standard working curve, Calculation results, or press the automatic Calculation results of linear equation.
When the inventive method is implemented, the deionized water consumption of washing molten sample wall of cup during the micro-wave digestion chromium carbide is preferably 1～2mL, adding purity more successively is that high-purity (MOS level), mass concentration are hydrofluorite 1.0～2.0mL of 1.14g/mL (grams per milliliter), adding purity is sulfuric acid 1.5～2.0mL that top grade is pure, mass concentration is 1.84g/mL, purity is that high-purity (MOS level), mass concentration are the nitric acid 0.8mL of 1.42g/mL, and mixing.
When the inventive method was implemented, twice micro-wave digestion running parameter was identical, is all: clear up that working pressure is followed successively by 2～3,5～6,8～9,11～12,14～15kg/cm each stage
2(kilograms per centimeter
2), corresponding each stage digestion time is followed successively by 120～150,150～180,320～360,300～330,220～250sec (second).
When the inventive method is implemented, need add the chromium matrix solution suitable when the aluminium of preparation chromium matrix coupling, calcium, iron, molybdenum, niobium, titanium, tungsten mixed standard solution series with test portion amount to be detected; When taking by weighing sample size was 0.1000 when gram, and the adding mass concentration is 17.3g/L (grams per liter) chromium matrix solution 5mL (milliliter); When taking by weighing sample size was 0.0500 when gram, and adding mass concentration is 17.3g/L chromium matrix solution 2.5mL.
Implement the analysis detecting data collection of the inventive method and result and calculate substantially that computing method are close as a result with conventional inductively coupled plasma atomic emission spectrometer data acquisition and conventional analysis, computational analysis testing result concrete grammar is:
1. look into standard working curve result of calculation as follows.
In the formula:
X represents tested element (aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten);
ρ represents the mass concentration that checks in tested element in the sample solution that blank correction is crossed on the standard working curve, (μ g/mL, mcg/ml);
V represents the volume of tested sample solution, (mL);
M represents the quality of test portion, (g).
2. the result is calculated and demonstrated to automatic data processing by following linear equation:
Linear equation: C=C
B+ KI
C by the mass concentration of mensuration sample solution, (μ g/mL);
C
BBy the mass concentration of mensuration sample solution background, (μ g/mL);
I by the emissive porwer of survey element
K is an equation coefficient
Advantage of the present invention is to adopt the acid mixture secondary microwave to clear up the chromium carbide sample, fundamentally solved the difficult technical barrier that decomposes of chromium carbide, make that impurity elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten become possibility in the analyzing and testing chromium carbide, thereby filled up the blank of impurities analysis detection method in the chromium carbide.And microwave digestion technology has fast, efficient, the digestion solution consumption is few, therefore characteristics such as background value is low are well suited for measuring micro impurity element, to the accuracy of measurement height of impurity elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide, precision is good, can satisfy the requirement of quality inspection.The impurity content scope that analyzing detecting method of the present invention is measured is 0.010%～1.00%, is highly suitable for the assay determination of impurity element in the chromium carbide, and the result is stable, consistent, favorable reproducibility.
Description of drawings
Fig. 1 is the standard working curve that the present invention measures with inductively coupled plasma atomic emission spectrometer.
Embodiment
Analyzing detecting method to seven kinds of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide of the present invention is described in further detail below.
1. standard solution preparation
Prepare aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten standard inventory solution that mass concentration is 1.000mg/mL (mg/ml) respectively, be stored in the plastic bottle.
The preparation mass concentration is aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution of 0.100mg/mL: pipette 10mL aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten standard inventory solution respectively in same 100mL (milliliter) plastics volumetric flask, adding purity successively is that high-purity (MOS level), mass concentration are the nitric acid 2mL of 1.42g/mL (grams per milliliter), purity is that high-purity (MOS level), mass concentration are the hydrofluorite 2.0mL of 1.14g/mL, be diluted to scale with deionized water, mixing is stored in the plastic bottle.
The preparation mass concentration is the chromium matrix solution of 17.3g/L (grams per liter): take by weighing 1.7330 gram crome metal (chromium content ω
Cr〉=99.9%) place the 200mL quartz beaker, adding purity is the pure sulfuric acid of top grade (1+1) 40mL, moves on on the electric hot plate, low-temperature heat is taken off cooling to dissolving fully, with deionized water purge wall of cup, move in the 100mL plastics volumetric flask, and be diluted to scale, mixing.
The mixed standard solution series of preparation chromium matrix coupling: pipette aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten mixed standard solution 0 that above-mentioned mass concentration is 0.100mg/mL respectively, 0.50mL, 1.00mL, 2.50mL, 5.00mL in one group of (5) 100mL plastics volumetric flask, (the concrete addition of chromium matrix solution should be suitable with test portion amount to be detected to add above-mentioned mass concentration and be chromium matrix solution 2.5～5.0mL of 17.3g/L (grams per liter), such as: when taking by weighing sample size was 0.1000 when gram, and adding mass concentration is 17.3g/L chromium matrix solution 5mL; When taking by weighing sample size was 0.0500 when gram, and adding mass concentration is 17.3g/L chromium matrix solution 2.5mL).Adding purity then is the pure sulfuric acid of top grade (1+1) 2mL, purity is that high-purity (MOS level), mass concentration are the nitric acid 0.8mL of 1.42g/mL, purity is that high-purity (MOS level), mass concentration are the hydrofluorite 2.0mL of 1.14g/mL, is diluted to scale with deionized water, mixing.Promptly be mixed with every mL (milliliter) and contain 0,0.50 μ g (microgram), 1.00 μ g, 2.50 μ g, aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of the chromium matrix coupling of 5.0 μ g.
2. by the step measurements drawing standard working curve of the inventive method or set up linear equation
The instrument condition of work that adopts the inventive method to measure impurity element in the chromium carbide on inductively coupled plasma atomic emission spectrometer is: generator power 950W (watt), cooling gas flow 12L/min (rise/minute), sheath airshed 0.3L/min, carrier gas flux 0.60～0.85L/min, height of observation 15mm (millimeter), entrance slit 10 μ m (micron), exit slit 15 μ m, 0.5sec integral time (second), reference line C193.026nm (nanometer), reference line high voltage parameter 700v (volt).The analysis of line wavelength of measuring each element in the chromium carbide under above-mentioned instrument condition of work is respectively: aluminium 394.401nm, calcium 396.847nm, iron 259.940nm, molybdenum 202.030nm, niobium 319.498nm, titanium 336.121nm, tungsten 239.709nm (wavelength following examples of instrument condition of work and element to be measured are all identical).
Under above condition of work, aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten mixed standard solution series that the chromium matrix that oneself is prepared mates are measured (carrying out blank determination simultaneously) on inductively coupled plasma atomic emission spectrometer, read the emissive porwer of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten, mass concentration with tested element is a horizontal ordinate, the emissive porwer of measuring is that ordinate is drawn out standard working curve (as Fig. 1) or with the mass concentration and the corresponding emissive porwer of serial mixed standard solution, set up aforementioned linear equation.
3. sample determination
Embodiment 1: the mensuration (sample S-1) of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide
Get 0.1000 gram chromium carbide test portion and place the molten sample cup of teflon, earlier with 1～2mL deionized water purge wall of cup, adding purity then successively is high-purity (MOS level, following examples are identical), mass concentration is the hydrofluorite 1.0mL of 1.14g/mL, purity is the sulfuric acid 1.5mL that top grade is pure, mass concentration is 1.84g/mL, purity is high-purity (MOS level, following examples are identical), mass concentration is the nitric acid 0.8mL of 1.42g/mL, mixing, cover bowl cover, and molten sample cup put into pressure pan, airtight pressure pan.Pressure pan is placed microwave dissolver, carry out the micro-wave digestion first time by condition of work shown in the table 1, after micro-wave digestion is finished for the first time pressure pan is shifted out from microwave dissolver, after treating the pressure pan cool to room temperature, again pressure pan is placed microwave dissolver to carry out the micro-wave digestion second time by clearing up same condition of work with the first time.
Table 1: microwave dissolver is cleared up the condition of work of chromium carbide
| Stage | Pressure (Kg/cm 2) | Time (S) |
| 1 | 3 | 120 |
| 2 | 6 | 180 |
| 3 | 9 | 360 |
| 4 | 12 | 300 |
| 5 | 15 | 240 |
Clear up finish after, take out pressure pan, treat that pressure pan cooling back opens jar in vent cabinet, take out molten sample cup and consoluet chromium carbide test solution moved in the 100mL plastics volumetric flask, be diluted to scale with deionized water, mixing.Under same above-mentioned instrument condition of work, aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of blank, chromium carbide test solution and chromium matrix coupling is measured simultaneously the emissive porwer of its element on inductively coupled plasma atomic emission spectrometer.
According to the emissive porwer of aluminium, calcium, iron, molybdenum, niobium, titanium, W elements in the chromium carbide test solution of measuring, find the mass concentration Calculation results of corresponding tested element by the automatic Calculation results of aforesaid linear equation or from aforesaid standard working curve (drawing when the adding mass concentration is 17.3g/L chromium matrix solution 5mL).To repeatedly measuring with a collection of chromium carbide sample, the mean value of analysis result, standard deviation, relative standard deviation see Table 2.
Table 2: analysis result and precision
| Element | Al | Ca | Fe | Mo | Nb | Ti | W |
| Measurement result mean value (%) | 0.038 | 0.042 | 0.068 | 0.039 | 0.010 | 0.019 | 0.024 |
| Standard deviation (%) | 0.0011 | 0.0012 | 0.0012 | 0.0018 | 0.0003 | 0.0006 | 0.0010 |
| Relative standard deviation (%) | 2.9 | 2.9 | 1.8 | 4.6 | 3.0 | 3.2 | 4.2 |
Embodiment 2: the mensuration (sample S-2) of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide
Get 0.1000 gram chromium carbide test portion and place the molten sample cup of teflon, earlier with 1～2mL deionized water purge wall of cup, adding purity then successively is hydrofluorite 1.5mL high-purity, that mass concentration is 1.14g/mL, purity is the sulfuric acid 2.0mL that top grade is pure, mass concentration is 1.84g/mL, purity is nitric acid 0.8mL high-purity, that mass concentration is 1.42g/mL, and mixing covers bowl cover, and molten sample cup put into pressure pan, airtight pressure pan.Pressure pan is placed microwave dissolver, carry out the micro-wave digestion first time by condition of work shown in the above-mentioned table 1, after micro-wave digestion is finished for the first time pressure pan is shifted out from microwave dissolver, after treating the pressure pan cool to room temperature, again pressure pan is placed microwave dissolver to carry out the micro-wave digestion second time by clearing up same condition of work with the first time.
Clear up finish after, take out pressure pan, treat that pressure pan cooling back opens jar in vent cabinet, take out molten sample cup and consoluet chromium carbide test solution moved in the 100mL plastics volumetric flask, be diluted to scale with deionized water, mixing.Under same above-mentioned instrument condition of work, aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of blank, chromium carbide test solution and chromium matrix coupling is measured simultaneously the emissive porwer of its element on inductively coupled plasma atomic emission spectrometer.
According to the emissive porwer of aluminium, calcium, iron, molybdenum, niobium, titanium, W elements in the chromium carbide test solution of measuring, find the mass concentration Calculation results of corresponding tested element by the automatic Calculation results of aforesaid linear equation or from aforesaid standard working curve (drawing when the adding mass concentration is 17.3g/L chromium matrix solution 5mL).To repeatedly measuring with a collection of chromium carbide sample, the mean value of analysis result, standard deviation, relative standard deviation see Table 3.
Table 3: analysis result and precision
| Element | Al | Ca | Fe | Mo | Nb | Ti | W |
| Measurement result mean value (%) | 0.010 | 0.013 | 0.034 | ＜0.010 | ＜0.010 | ＜0.010 | 0.015 |
| Standard deviation (%) | 0.0005 | 0.0007 | 0.0008 | - | - | - | 0.0007 |
| Element | Al | Ca | Fe | Mo | Nb | Ti | W |
| Relative standard deviation (%) | 5.0 | 5.4 | 1.8 | - | - | - | 4.7 |
Embodiment 3: the mensuration (sample S-3) of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide
Get 0.1000 gram chromium carbide test portion and place the molten sample cup of teflon, earlier with 1～2mL deionized water purge wall of cup, adding purity then successively is hydrofluorite 2.0mL high-purity, that mass concentration is 1.14g/mL, purity is the sulfuric acid 2.0mL that top grade is pure, mass concentration is 1.84g/mL, purity is nitric acid 0.8mL high-purity, that mass concentration is 1.42g/mL, and mixing covers bowl cover, and molten sample cup put into pressure pan, airtight pressure pan.Pressure pan is placed microwave dissolver, carry out the micro-wave digestion first time by condition of work shown in the table 4, after micro-wave digestion is finished for the first time pressure pan is shifted out from microwave dissolver, after treating the pressure pan cool to room temperature, again pressure pan is placed microwave dissolver to carry out the micro-wave digestion second time by clearing up same condition of work with the first time.
Table 4: microwave dissolver is cleared up the condition of work of chromium carbide
| Stage | Pressure (Kg/cm 2) | Time (S) |
| 1 | 3 | 150 |
| 2 | 5 | 150 |
| 3 | 8 | 320 |
| 4 | 11 | 330 |
| 5 | 14 | 250 |
Clear up finish after, take out pressure pan, treat that pressure pan cooling back opens jar in vent cabinet, take out molten sample cup and consoluet chromium carbide test solution moved in the 100mL plastics volumetric flask, be diluted to scale with deionized water, mixing.Under same above-mentioned instrument condition of work, aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of blank, chromium carbide test solution and chromium matrix coupling is measured simultaneously the emissive porwer of its element on inductively coupled plasma atomic emission spectrometer.
According to the emissive porwer of aluminium, calcium, iron, molybdenum, niobium, titanium, W elements in the chromium carbide test solution of measuring, find the mass concentration Calculation results of corresponding tested element by the automatic Calculation results of aforesaid linear equation or from aforesaid standard working curve (drawing when the adding mass concentration is 17.3g/L chromium matrix solution 5mL).Because some impurity content is less than 0.010% in most of chromium carbide samples, for precision and the accuracy check of carrying out method at impurity content under greater than 0.010% condition, take by weighing with a collection of chromium carbide sample, add a certain amount of aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten mixed standard solution respectively, carry out mark-on and reclaim experiment, repeatedly measure by the sample determination step, the mean value of Calculation results, standard deviation, relative standard deviation and the recovery, data see Table 5.
Table 5: analysis result, precision and determination of recovery rates result
| Element | Al | Ca | Fe | Mo | Nb | Ti | W |
| Measurement result mean value (%) | 0.030 | 0.033 | 0.055 | 0.025 | 0.028 | 0.026 | 0.035 |
| Standard deviation (%) | 0.0009 | 0.0011 | 0.0010 | 0.0013 | 0.0008 | 0.0009 | 0.0015 |
| Relative standard deviation (%) | 3.0 | 3.3 | 1.8 | 5.2 | 2.9 | 3.5 | 4.3 |
| Average recovery rate (%) | 104.5 | 101.5 | 96.0 | 97.5 | 103.5 | 102.0 | 94.5 |
Embodiment 4: the mensuration (sample S-4) of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide
Get 0.0500 gram chromium carbide test portion and place the molten sample cup of teflon, earlier with 1～2mL deionized water purge wall of cup, adding purity then successively is hydrofluorite 1.0mL high-purity, that mass concentration is 1.14g/mL, purity is the sulfuric acid 1.5mL that top grade is pure, mass concentration is 1.84g/mL, purity is nitric acid 0.8mL high-purity, that mass concentration is 1.42g/mL, and mixing covers bowl cover, and molten sample cup put into pressure pan, airtight pressure pan.Pressure pan is placed microwave dissolver, carry out the micro-wave digestion first time by condition of work shown in the table 6, after micro-wave digestion is finished for the first time pressure pan is shifted out from microwave dissolver, after treating the pressure pan cool to room temperature, again pressure pan is placed microwave dissolver to carry out the micro-wave digestion second time by clearing up same condition of work with the first time.
Table 6: microwave dissolver is cleared up the condition of work of chromium carbide
| Stage | Pressure (Kg/cm 2) | Time (S) |
| 1 | 2 | 120 |
| 2 | 5 | 150 |
| 3 | 8 | 320 |
| 4 | 11 | 300 |
| 5 | 14 | 220 |
Clear up finish after, take out pressure pan, treat that pressure pan cooling back opens jar in vent cabinet, take out molten sample cup and consoluet chromium carbide test solution moved in the 100mL plastics volumetric flask, be diluted to scale with deionized water, mixing.Under same above-mentioned instrument condition of work, aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution series of blank, chromium carbide test solution and chromium matrix coupling is measured simultaneously the emissive porwer of its element on inductively coupled plasma atomic emission spectrometer.
According to the emissive porwer of aluminium, calcium, iron, molybdenum, niobium, titanium, W elements in the chromium carbide test solution of measuring, find the mass concentration Calculation results of corresponding tested element by the automatic Calculation results of aforesaid linear equation or from aforesaid standard working curve (drawing when the adding mass concentration is 17.3g/L chromium matrix solution 2.5mL).Because impurity content is all less than＜0.50% in most of chromium carbide samples, but also there is impurity content high slightly, for to impurity content at 0.50%～1.00% o'clock, carry out the precision and the accuracy check of method, take by weighing with a collection of chromium carbide sample, add a certain amount of aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten mixed standard solution respectively, carry out mark-on and reclaim experiment, repeatedly measure by the sample determination step, the mean value of Calculation results, standard deviation, relative standard deviation and the recovery, data see Table 7.
Table 7: analysis result, precision and determination of recovery rates result
| Element | Al | Ca | Fe | Mo | Nb | Ti | W |
| Measurement result mean value (%) | 0.82 | 0.84 | 0.84 | 0.81 | 0.81 | 0.81 | 0.83 |
| Standard deviation (%) | 0.015 | 0.018 | 0.015 | 0.022 | 0.016 | 0.013 | 0.021 |
| Relative standard deviation (%) | 1.8 | 2.1 | 1.8 | 2.7 | 2.0 | 1.6 | 2.5 |
| Average recovery rate (%) | 99.3 | 103.0 | 102.0 | 105.7 | 98.5 | 99.5 | 98.0 |
Above embodiment explanation: according to the analyzing detecting method of seven kinds of elements such as aluminium, calcium, iron, molybdenum, niobium, titanium, tungsten in the chromium carbide of the present invention, sample is carried out mark-on reclaim experiment, the recovery is all between 94.5%～105.7%; Sample is carried out independent mensuration more than five times, and the relative standard deviation of method illustrates that all less than 5.4% the inventive method has good accuracy and precision, is accurately feasible.
Claims (4)
1. the analyzing detecting method of impurity element aluminium, calcium, iron, molybdenum, niobium, titanium and tungsten in the chromium carbide comprises the steps:
(1) the chromium carbide test portion is placed the molten sample cup of teflon, behind deionized water purge wall of cup, add hydrofluorite, sulfuric acid, nitric acid successively, mixing covers bowl cover, and molten sample cup is put into airtight pressure pan;
(2) pressure pan is placed microwave dissolver, the selected working pressure of mode and the digestion time that increase progressively stage by stage by working pressure carry out the micro-wave digestion first time continuously, after clearing up and finish the first time pressure pan is shifted out and cool to room temperature, and then place microwave dissolver to carry out the micro-wave digestion second time pressure pan by clearing up same condition of work with the first time;
(3) from microwave dissolver, take out pressure pan, open jar after the cooling, consoluet chromium carbide test solution is moved in the plastics volumetric flask, be diluted to scale with deionized water, mixing;
(4) the standard solution series of the aluminium of preparation chromium matrix coupling, calcium, iron, molybdenum, niobium, titanium, tungsten mixing;
(5) under selected instrument condition of work, with the serial emissive porwer of on inductively coupled plasma atomic emission spectrometer, measuring aluminium, calcium, iron, molybdenum, niobium, titanium, W elements simultaneously of the mixed standard solution of blank, chromium carbide test solution and preparation, Calculation results then.
2. the analyzing detecting method of impurity element aluminium, calcium, iron, molybdenum, niobium, titanium and tungsten in the chromium carbide according to claim 1, the deionized water consumption of washing molten sample wall of cup when it is characterized in that the micro-wave digestion chromium carbide is 1～2 milliliter, add purity more successively and be 1.0～2.0 milliliters in the hydrofluorite high-purity, that mass concentration is 1.14 grams per milliliters, add purity and be 1.5～2.0 milliliters in the sulfuric acid that top grade is pure, mass concentration is 1.84 grams per milliliters, purity is 0.8 milliliter in high-purity, that mass concentration is 1.42 grams per milliliters nitric acid, and mixing.
3. the analyzing detecting method of impurity element aluminium, calcium, iron, molybdenum, niobium, titanium and tungsten in the chromium carbide according to claim 1, it is characterized in that twice micro-wave digestion running parameter is: each stage clears up working pressure and is followed successively by 2～3,5～6,8～9,11～12,14～15 kilograms per centimeter
2, corresponding each stage digestion time was followed successively by 120～150,150～180,320～360,300～330,220～250 seconds.
4. the analyzing detecting method of impurity element aluminium, calcium, iron, molybdenum, niobium, titanium and tungsten in the chromium carbide according to claim 1, the aluminium, calcium, iron, molybdenum, niobium, titanium, the tungsten mixed standard solution that it is characterized in that preparing chromium matrix coupling need add the chromium matrix solution suitable with test portion amount to be detected when serial, when taking by weighing sample size was 0.0500～0.1000 when gram, and adding mass concentration is 2.5～5 milliliters of 17.3 grams per liter chromium matrix solution.
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