CN100498309C - Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method - Google Patents
Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method Download PDFInfo
- Publication number
- CN100498309C CN100498309C CNB031264360A CN03126436A CN100498309C CN 100498309 C CN100498309 C CN 100498309C CN B031264360 A CNB031264360 A CN B031264360A CN 03126436 A CN03126436 A CN 03126436A CN 100498309 C CN100498309 C CN 100498309C
- Authority
- CN
- China
- Prior art keywords
- sample
- standard
- metal
- content
- quality
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to a method for analyzing metal elements in catalytic cracking catalyst by utilizing X-ray fluorescence method. Said method is characterized by that firstly, 8-14 standard samples with different metal contents can be prepared, the described standard sample is metal oxide loaded on the carrier, in which the carrier is formed from 60-80 mass% of aluminium oxide and 20-40 mass% of silicon oxide, and the described metal includes iron, sodium, mixed rare earth, nickel, copper, vanadium, antimony and calcium, then the standard sample can be tabletted, and a metal content determination empirical formula can be created, so that said invention can utilizes determination of X-ray fluorescence intensity of every metal element in the sample to be tested and utilizes the empirical formula of every metal element to obtain the content of every metal in said sample.
Description
Technical field
The present invention is a method of utilizing the x-ray fluorescence method analysis of catalyst to form, specifically, is a kind of method of utilizing x-ray fluorescence method to analyze metal component content in the catalytic cracking catalyst.
Background technology
Along with the development of oil deep processing, the feedstock oil that uses in heavy oil, the RCC technology tends to heaviness, poor qualityization gradually, causes contained heavy metal in the oil that the pollution of catalyzer is become increasingly conspicuous.Verified, a small amount of even trace heavy metals, particularly metallic nickel and vanadium ion in the charging seriously influence the performance of catalyzer.The aluminium oxide effect forms low-melting fused matter in vanadium metal and the catalyzer, almost all is deposited on the catalyst surface.In the catalyst aging process, it can slowly be moved near the molecules of active components sieve, and molecular sieve structure is destroyed.Metallic nickel can be accelerated the dehydrogenation reaction of hydro carbons under cracking conditions.Therefore, the existence of heavy metal descends activity of such catalysts, selectivity, product distribution variation, and gasoline and liquefied gas yield descend, and dry gas and coke productive rate rise.For in time the day of decision FCC catalysts is unloaded output, improve the working ability of catalytic cracking unit, guarantee the yield of high value lightweight oil, increase economic efficiency, the variation of contents of heavy metal elements and active metal constituent content on the monitoring catalyst in time.
Methods such as many in the past employing atomic emission spectrums, atomic absorption are carried out control analysis to the metallic element in the Cracking catalyst.Rare earth in the catalyzer and heavy metal need to measure respectively, and need specimen be dissolved with strong acid, the sample preparation complex operation, analysis speed is slower, sample of each measurement needs 4 hours at least, can not satisfy the needs that scientific research and commercial production are carried out express-analysis.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing x-ray fluorescence method to measure metal element content in the catalytic cracking catalyst, this method can be measured the content of multiple metallic element in the catalyzer, and is fast, accurately, easy to operate.
The method of utilizing x-ray fluorescence method to analyze metallic element in the catalytic cracking catalyst provided by the invention comprises the steps:
(1) preparation standard sample: 8-14 standard model of preparation with different metal content, described standard model is the metal oxide that loads on the carrier, wherein carrier is made up of the aluminium oxide of 60-80 quality % and the monox of 20-40 quality %, described metal is iron, sodium, mishmetal, nickel, copper, vanadium, antimony and calcium, La in the described mishmetal
2O
3: CeO
2: Pr
6O
11; Nd
2O
3Mass ratio be 45:40:5:10, contained metal oxide except that mixed rare-earth elements in the content of metal is in each standard model:
RE
2O
30.7-3.5 quality %, Fe 0.1-2.0 quality %, Na 0.2-1.4 quality %, Ni 0.1-2.0 quality %, Cu 0.01-0.20 quality %, V 0.05-1.4 quality %, Sb 0.01-0.50 quality %, Ca 0.1-2.5 quality %,
(2) standard sample compressing tablet: the standard model with different metal content that will prepare, each sample are got the 1.0-2.0 gram, with the 2000-8000 kg/cm
2Pressure compacting in flakes,
(3) set up tenor and measure empirical formula: the spectral strength of measuring contained metallic element in each standard sample with the x-ray fluorescence spectrometry instrument, try to achieve standard equation constant and the correction coefficient of measuring element in the empirical formula by least square method, set up the empirical equation that each metal element content is measured
(4) sample determination: the method compressing tablet of testing sample being pressed standard sample, and under the condition identical, carry out x-ray fluorescence and measure with the standard sample test condition, by the spectral strength of each metallic element of testing sample, the empirical formula that each metal element content of being set up by (3) step is measured is tried to achieve the content of contained each metal in the sample.
The present invention adopts x-ray fluorescence to measure the content of metallic element in the Cracking catalyst, only need in the operation the simple compressing tablet of sample can directly be measured, operate comparatively simple, measure fast, accurately, sample of single measurement only needs 20 minutes, can satisfy the needs of refinery's on-line analysis and laboratory routine analysis well.
Embodiment
The key of measuring catalyst metal content with the inventive method is to prepare several standard samples suitable with the testing sample chemical composition, constituent content in the standard sample carrier should be suitable with the contained element of catalyst substrates material to be measured, as, the active component of catalytic cracking catalyst is a Y zeolite, wherein also contain cementing agent, they all are sieve and silica-sesquioxides.Therefore, the standard sample carrier also will be with the preparation of the potpourri of monox and aluminium oxide, and regulates the two ratio, makes the content of these two kinds of materials in itself and the catalyzer suitable.Otherwise, will produce matrix effect during test, accuracy is measured in influence.Institute's containing metal and content thereof are also suitable with the metal and the content that easily adhere on it in institute's containing metal in the catalyzer and its use in the standard sample.That is to say that the metal that contains in the standard sample should be more than the metal that contains in the testing sample, the content range of each metal should be greater than the fluctuation range of tenor in the testing sample in the standard sample.
The preparation method of standard sample is among the present invention: earlier aluminium oxide and the monox mass ratio by 6-8:2-4 is mixed, then at 800-900 ℃ of roasting 1-3 hour, add and press La in advance
2O
3: CeO
2: Pr
6O
11: Nd
2O
3Mass ratio is the mixed rare-earth oxide that 45:40:5:10 prepares, the standard solution that adds iron, sodium, nickel, copper, vanadium, antimony and the calcium of scheduled volume again, after the drying, add the absolute ethyl alcohol ground and mixed to even, 800-900 ℃ roasting 1-3 hour, the aqueous solution of the titer of described iron and nickel for making behind each metal and the nitric acid reaction, the titer of copper are the aqueous solution that CuO makes after with the nitric acid heating for dissolving, and the titer of vanadium is V
2O
5With the aqueous solution that the strong aqua heating for dissolving makes, the titer of sodium is the aqueous solution of NaC1, and the titer of antimony is Sb
2O
3With the aqueous solution that the concentrated hydrochloric acid heating for dissolving makes, the titer of calcium is CaCO
3With the aqueous solution that makes behind the dissolving with hydrochloric acid.Preparation iron, nickel, the used preferred 1:1 nitric acid of nitric acid of copper titer, the hydrochloric acid of the preferred 1:1 of hydrochloric acid that preparation standard calcium liquid is used.
In the titer of above-mentioned preparation, the concentration of standard solution of iron, sodium, nickel and calcium is the 8-12 mg/ml, and the concentration of standard solution of copper, vanadium and antimony is the 2-5 mg/ml.
The used material of preparation standard sample will have high purity, and the used aluminium oxide of preparation carrier is analysis pure sample product, and monox purity is 99.9%.Used various oxides and the salt of preparation titer is spectroscopic pure, and the iron wire of use and nickel sheet purity all should be higher than 99.9%.During preparation various material dosages accurately weighing to precision be no more than 0.2 ‰.
Each titer cumulative volume that above-mentioned preparation standard sample adds is 5-9:1 with the liquid of carrier/solid volume ratio, and the carrier drying after the adding titer is ground to the single-size that particle diameter is the 70-80 micron.Add absolute ethyl alcohol during grinding as lubricant, the addition of absolute ethyl alcohol is 0.8-2.0 a times of solid masses.After treating in the sample ethanol volatilization fully, with sample 800-900 ℃ of roasting.
After the sample that makes after the roasting is wanted compressing tablet, could use the x-ray fluorescence instrument to measure.The sample size that compressing tablet uses restrains as 1.0-2.0, and standard sample is put into the aluminum sample box, is pressed into diaphragm seal with the high pressure of 2000-10000 kg/cm 2.
The present invention adopts empirical formula to predict tenor in the catalyzer to be measured, and therefore, the standard sample of preparation is many more, and the empirical formula of foundation is accurate more.Generally need the standard sample of preparation more than 8, the various tenors in each standard sample are all inequality, random variation in the content range of its regulation.
After standard sample makes, measure the spectral strength of each metallic element with the x-ray fluorescence instrument, condition determination is: end window rhodium target, 50 kilovolts of voltages, 50 milliamperes in electric current, thick collimating apparatus, vacuum light path.Each metallic element is selected certain wave height scope according to the character of its characteristic peak, and spectral strength is calculated, concrete condition determination such as table 1.
Table 1
In the inventive method, (3) step is an empirical formula of setting up each tenor by the standard sample test result.Empirical coefficient method is the most frequently used Mathematical Correction Method, and the empirical equation of various ways is arranged.The empirical formula equation that the present invention adopts is W
i=W
i' (1+ ∑ A
IjW
j'), W wherein
i'=aI
i 2+ bI
i+ c,
In the formula, W
iBe the content of mensuration metallic element i,
W
i' be the apparent content of measuring metallic element i,
W
j' be the apparent content of metallic element j in the standard sample,
I
iBe the spectral strength of mensuration metallic element i,
A
IjBe the factor of metallic element j in the standard sample, or claim matrix element j correction coefficient mensuration element i to mensuration metallic element i influence,
A, b, c are the standard equation constant.
Adopt least square method to be by the method for standard sample test data basis of calculation equation constant:
X-ray fluorescence spectral strength when measuring earlier each metallic element different content in the standard model that an assembly makes is with known content value (massfraction) the substitution standard equation W of metal in the intensity that records and the standard model
i'=aI
i 2+ bI
iAmong+the c, obtain curve constant a, b and the c of each metallic element with least square method.Thus, record the intensity of testing sample metallic element i after, can calculate the apparent content W of metallic element i in the sample by standard equation
i'.
The major metal component that catalytic cracking catalyst need be measured is rare earth element, iron and sodium, after catalyzer uses, can contain pollution element copper, nickel, vanadium, antimony and calcium, the existence meeting of rare earth element exerts an influence to the mensuration of other element, form more serious matrix effect, also have between other heavy metal and influence each other.Therefore, try to achieve the apparent content of each element in the sample by standard equation after, also to determine other element in the sample to measuring the correction coefficient of element, the apparent content of the metallic element measured is carried out coefficient correction, just can obtain measurement result accurately.
Correction coefficient A
IjAssay method be: record the apparent concentration when the variable concentrations of each element in the standard specimen group by experiment, the apparent concentration of measuring element in the sample be made as W
i', the apparent concentration of other element is made as W
j', with they substitution equation W
i=W
i' (1+ ∑ A
IjW
j') in, can list the equation identical to each element with the standard specimen number, use least square method can obtain A
Ij, each matrix element j is long-pendingly added and is ∑ A the apparent concentration of the correction coefficient of measuring element i and matrix element is
IjW
j'.
In addition, with the sodium content in the standard specimen mensuration catalyst sample of preparation, owing to there is structure effect, have than mistake, therefore, the correction coefficient of sodium also needs with the catalyst sample that accurate content is arranged the typical curve of sodium further to be proofreaied and correct and got except carrying out matrix correction.
When using the inventive method specimen, do not need roasting, only need be ground into the particle that particle diameter is the 70-80 micron, can pack in the sample box, with the identical condition lower sheeting of preparation standard sample, adjust the instrument test condition, with the identical condition of bioassay standard sample under test, with the spectral strength substitution standard equation of each metallic element of recording, try to achieve the apparent content of each metal, again with apparent content substitution W
i=W
i' (1+ ∑ A
IjW
j') in, can try to achieve the content of each metallic element.
Before specimen, drift preferably rectifies an instrument earlier.Method is to select 1 or 2 standard model that tested constituent content is moderate in standard specimen series, measures the wherein peak intensity of each metallic element, deposits computing machine in.During measuring samples, measure the standard model of known content earlier, the instrument drift amount is adjusted to zero, and then working sample.
Below by example in detail the present invention, but the present invention is not limited to this.
Example 1
This examples preparation standard sample.
(1) preparation carrier: with high-purity Al
2O
3(analyzing pure 4N, the Beijing Chemical Plant) and high-purity Si O
2(purity is 99.9%, Shanghai chemical reagent work) mixes by the mass ratio of 7:3, and the standard sample carrier is made in 850 ℃ of calcinations 1 hour.
(2) preparation titer
Mixed rare-earth oxide: with spectroscopic pure rare earth oxide La
2O
3, CeO
2, Pr
6O
11, Nd
2O
3Ratio in 45:40:5:10 mixes, and is made into mixed rare-earth oxide.
Fe standard solution (10 mg/ml): accurately taking by weighing purity is 99.9% metal iron wire, 2 grams (claiming accurate to ± 0.0002 gram), with 1: 1 nitric acid dissolve, is diluted to 200 milliliters with deionized water.
Ni standard solution (10 mg/ml): accurately taking by weighing purity is 99.99% metallic nickel sheet, 2 grams (claiming accurate to ± 0.0002 gram), with 1: 1 nitric acid dissolve, is diluted to 200 milliliters with deionized water.
Cu standard solution (3 mg/ml): accurately take by weighing 1 hour spectroscopic pure CuO0.75 of 120 ℃ of dryings gram (claiming accurate),, be diluted to 200 milliliters with deionized water with 1: 1 nitric acid heating for dissolving to ± 0.0002 gram.
V standard solution (3 mg/ml): accurately take by weighing 1 hour spectroscopic pure V of 120 ℃ of dryings
2O
51.0712 gram (claiming accurate to ± 0.0002 gram) is used the strong aqua heating for dissolving, is diluted to 200 milliliters with 1:9 ammoniacal liquor.
Sb standard solution (3 mg/ml): accurately take by weighing 1 hour spectroscopic pure Sb of 120 ℃ of dryings
2O
30.7219 gram (claiming accurate to ± 0.0002 gram) is used the concentrated hydrochloric acid heating for dissolving, is diluted to 200 milliliters with 1:9 hydrochloric acid.
Ca standard solution (10 mg/ml): accurately take by weighing 1 hour spectroscopic pure CaCO of 120 ℃ of dryings
3Gram (claiming accurate to ± 0.0002 gram) with 1: 1 dissolving with hydrochloric acid, is diluted to 200 milliliters with deionized water.
Na standard solution (10 mg/ml): accurately take by weighing 1 hour spectroscopic pure NaCl5.0870 of 120 ℃ of dryings gram (claiming accurate), with deionized water dissolving and be diluted to 200 milliliters to ± 0.0002 gram.
(3) preparation standard sample
Get 2.8239 gram carriers, first predetermined amounts adds rare earth oxide 0.0300 gram, and predetermined amounts adds the titer of other metal of (2) step preparation again, and the titer cumulative volume of adding is 15.1 milliliters.Under infrared lamp sample is dried, it is even to add 2.5 milliliters of absolute ethyl alcohol ground and mixed, 850 ℃ of roastings 1 hour.The metal element content of each standard sample sees Table 2.The series standard sample that makes is respectively got 1.5 grams, put into the aluminum sample box, in 5000 kg/cm
2Pressure to depress to diameter be 25 millimeters disk.
Example 2
Set up the standard equation that tenor is measured, determine correction coefficient.
With the standard sample that example 1 makes, test by the condition of table 1 one by one, with the peak intensity substitution standard equation that records, try to achieve the constant of each tenor bioassay standard equation, list in table 3.
With the peak intensity value of each standard sample of different metal content, the substitution standard equation is tried to achieve the apparent content of metallic element in each standard sample, again with its substitution W
i=W
i' (1+ ∑ A
IjW
j') in, every kind of element is listed ten equations, try to achieve matrix element the correction coefficient of measuring element is seen Table 4.The lookup method of correction coefficient is in the table 4: walking crosswise the selected metallic element i that measures, determine matrix effect element j in stringer more earlier, two row intersections are matrix element j to measuring the correction coefficient of element.
Example 3
Get the catalytic cracking catalyst that ten refinerys were used, it is ground to particle diameter is 74 microns particle.Get the catalyzer after 1.5 grams grind, put into sample box, be pressed into 16 disks, place instrument to measure each sample by the condition of table 1 by the method for example 1, with the peak intensity value substitution empirical formula of different metal element in each sample, the metal element content that calculates in each sample sees Table 5.
As shown in Table 5, the measurement result basically identical of the inventive method measurement result and other reference analytical approach.
Example 4
Investigate the inventive method precision.
Get a catalyst sample, be pressed into 11 disks, carry out repeatability and measure, the results are shown in Table 6.Other gets a catalyst sample, and compacting different timing 11 times, the results are shown in Table 7 in flakes.By table 6, table 7 as can be known, the relative standard deviation of the present invention's mensuration is less than 2%.
Example 5
Measure the metal element content in the fresh catalytic cracking catalyst.
Get freshly prepd rare-earth element modified fresh catalytic cracking catalyst, it is ground to particle diameter is 74 microns particle.Get the catalyzer after 1.5 grams grind, put into sample box, be pressed into disk by the method for example 1, place the measuring condition working sample of instrument by table 1, with the peak intensity value substitution empirical formula of different metal element in the sample, the content that calculates each element sees Table 8.Reference method listed in the table 8 is identical with table 5.
Table 2
Table 3
Table 4
Table 5
Annotate: the contrast of the result of 1 Fe.Ni.Cu.V.Sb.Ca and ICP (emission spectrum) method.
The contrast of the result of 2 Na and AAS (atomic absorption) method.
3 RE
2O
3Result and colourimetry contrast.
Table 6
Table 7
Table 8
Claims (8)
1, a kind of method of utilizing x-ray fluorescence method to analyze tenor in the catalytic cracking catalyst comprises the steps:
(1) preparation standard sample: 8-14 standard model of preparation with different metal content, described standard model is the metal oxide that loads on the carrier, wherein carrier is made up of the aluminium oxide of 60-80 quality % and the monox of 20-40 quality %, described metal is iron, sodium, mishmetal, nickel, copper, vanadium, antimony and calcium, La in the described mishmetal
2O
3: CeO
2: Pr
6O
11: Nd
2O
3Mass ratio be 45: 40: 5: 10, contained metal oxide except that mixed rare-earth elements in the content of metal is in each standard model:
RE
2O
30.7-3.5 quality %, Fe0.1-2.0 quality %, Na0.2-1.4 quality %, Ni0.1-2.0 quality %, Cu0.01-0.20 quality %, V0.05-1.4 quality %, Sb0.01-0.50 quality %, Ca0.1-2.5 quality %,
(2) standard sample compressing tablet: the standard model with different metal content that will prepare, each sample are got the 1.0-2.0 gram, with the 2000-10000 kg/cm
2Pressure compacting in flakes,
(3) set up tenor and measure empirical formula: the spectral strength of measuring contained metallic element in each standard sample with the x-ray fluorescence spectrometry instrument, try to achieve standard equation constant and the correction coefficient of measuring element in the empirical formula by least square method, set up the empirical equation that each metal element content is measured
(4) sample determination: the method compressing tablet of testing sample being pressed standard sample, and under the condition identical, carry out the x-ray fluorescence strength detection with the standard sample test condition, by the spectral strength of each metallic element of testing sample, the empirical formula of each metallic element of being set up by (3) step is tried to achieve the content of contained each metal in the sample.
2, in accordance with the method for claim 1, it is characterized in that (3) go on foot the empirical formula of setting up is W
i=W
i' (1+ ∑ A
IjW
j'), W wherein
i'=aI
i 2+ bI
i+ c, in the formula, W
iFor measuring the content of metallic element i, W
i' for measuring the apparent content of metallic element i, I
iFor measuring the spectral strength of metallic element i, A
IjBe the correction coefficient of metallic element j in the standard sample to mensuration metallic element i influence, W
j' be the apparent content of metallic element j in the standard sample, a, b, c are the standard equation constant.
3, in accordance with the method for claim 1, it is characterized in that the preparation method of described standard sample is: earlier aluminium oxide and the monox mass ratio by 6-8: 2-4 is mixed, then at 800-900 ℃ of roasting 1-3 hour, La is pressed in adding in advance again
2O
3: CeO
2: Pr
6O
11: Nd
2O
3Mass ratio is 45: 40: 5: 10 mixed rare-earth oxides that prepare, the standard solution that adds iron, sodium, nickel, copper, vanadium, antimony and the calcium of scheduled volume again, after the drying, add the absolute ethyl alcohol ground and mixed to even, 800-900 ℃ roasting 1-3 hour, the aqueous solution of the titer of described iron and nickel for making behind each metal and the nitric acid reaction, the titer of copper are the aqueous solution that CuO makes after with the nitric acid heating for dissolving, and the titer of vanadium is V
2O
5With the aqueous solution that the strong aqua heating for dissolving makes, the titer of sodium is the aqueous solution of NaCl, and the titer of antimony is Sb
2O
3With the aqueous solution that the concentrated hydrochloric acid heating for dissolving makes, the titer of calcium is CaCO
3With the aqueous solution that makes behind the dissolving with hydrochloric acid.
4, in accordance with the method for claim 3, the concentration of standard solution that it is characterized in that iron, sodium, nickel and calcium is the 8-12 mg/ml, and the concentration of standard solution of copper, vanadium and antimony is the 2-5 mg/ml.
5, in accordance with the method for claim 3, the absolute ethyl alcohol that adds when it is characterized in that grinding be solid masses 1-2 doubly.
6, in accordance with the method for claim 3, it is characterized in that adding that to be ground to solid grain size behind the absolute ethyl alcohol be the 70-80 micron.
7, in accordance with the method for claim 1, it is characterized in that described x-ray fluorescence condition determination is: end window rhodium target, 50 kilovolts of voltages, 50 milliamperes in electric current, thick collimating apparatus, vacuum light path.
8, in accordance with the method for claim 1, it is characterized in that standard sample puts into the aluminum sample box and be pressed into diaphragm seal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031264360A CN100498309C (en) | 2003-09-28 | 2003-09-28 | Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031264360A CN100498309C (en) | 2003-09-28 | 2003-09-28 | Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1601261A CN1601261A (en) | 2005-03-30 |
| CN100498309C true CN100498309C (en) | 2009-06-10 |
Family
ID=34658800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031264360A Expired - Lifetime CN100498309C (en) | 2003-09-28 | 2003-09-28 | Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100498309C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8664595B2 (en) | 2012-06-28 | 2014-03-04 | Fei Company | Cluster analysis of unknowns in SEM-EDS dataset |
| US8880356B2 (en) | 2008-02-06 | 2014-11-04 | Fei Company | Method and system for spectrum data analysis |
| US8937282B2 (en) | 2012-10-26 | 2015-01-20 | Fei Company | Mineral identification using mineral definitions including variability |
| US9048067B2 (en) | 2012-10-26 | 2015-06-02 | Fei Company | Mineral identification using sequential decomposition into elements from mineral definitions |
| US9091635B2 (en) | 2012-10-26 | 2015-07-28 | Fei Company | Mineral identification using mineral definitions having compositional ranges |
| US9188555B2 (en) | 2012-07-30 | 2015-11-17 | Fei Company | Automated EDS standards calibration |
| US9194829B2 (en) | 2012-12-28 | 2015-11-24 | Fei Company | Process for performing automated mineralogy |
| US9714908B2 (en) | 2013-11-06 | 2017-07-25 | Fei Company | Sub-pixel analysis and display of fine grained mineral samples |
| US9778215B2 (en) | 2012-10-26 | 2017-10-03 | Fei Company | Automated mineral classification |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7490009B2 (en) | 2004-08-03 | 2009-02-10 | Fei Company | Method and system for spectroscopic data analysis |
| CN101799437B (en) * | 2009-02-06 | 2011-12-07 | 中国石油天然气股份有限公司 | Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method |
| CN101776622B (en) * | 2009-12-29 | 2012-06-13 | 聚光科技(杭州)股份有限公司 | Soil measuring method |
| CN103575581A (en) * | 2013-07-25 | 2014-02-12 | 葛洲坝集团水泥有限公司 | Element detection standard sample preparation and application methods |
| EP2894463A1 (en) * | 2014-01-13 | 2015-07-15 | PANalytical B.V. | Method of making a dry reference standard for X-ray fluorescence measurements |
| CN105784745B (en) * | 2014-12-24 | 2019-06-07 | 中国石油天然气股份有限公司 | A kind of method of nickel element content in measurement hydrogenation catalyst |
| CN104865285A (en) * | 2015-05-20 | 2015-08-26 | 中华人民共和国防城港出入境检验检疫局 | Method for rapidly determining aluminum species in dried beancurd sticks by adopting X-ray fluorescence spectrometer |
| CN105136832A (en) * | 2015-09-09 | 2015-12-09 | 重庆长安工业(集团)有限责任公司 | Detection method for TiO2, V2O5, WO3 in metallic oxide catalyst |
| CN105388141A (en) * | 2015-12-23 | 2016-03-09 | 中国科学院兰州化学物理研究所 | Method for measuring gold element content in core-shell type gold-magnetic nano composite catalyst through inductively coupled plasma emission spectrum |
| CN106370686A (en) * | 2016-08-31 | 2017-02-01 | 广西出入境检验检疫局危险品检测技术中心 | Method for determining copper content in basic copper carbonate for fireworks and firecrackers |
| CN106226340A (en) * | 2016-08-31 | 2016-12-14 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate |
-
2003
- 2003-09-28 CN CNB031264360A patent/CN100498309C/en not_active Expired - Lifetime
Non-Patent Citations (8)
| Title |
|---|
| X射线荧光光谱法测定重整催化剂中铂、铕、铈. 高萍等.分析试验室，第21卷第6期. 2002 |
| X射线荧光光谱法测定重整催化剂中铂、铕、铈. 高萍等.分析试验室，第21卷第6期. 2002 * |
| 催化裂化催化剂上污染重金属含量测定的XRF光谱分析方法的研究. 顾若晶等.光散射学报，第12卷第4期. 2001 |
| 催化裂化催化剂上污染重金属含量测定的XRF光谱分析方法的研究. 顾若晶等.光散射学报，第12卷第4期. 2001 * |
| 加氢催化剂中稀土及钼、钴含量的X射线荧光光谱测定方法的研究. 高萍等。.光谱学与光谱分析，第23卷第3期. 2003 |
| 加氢催化剂中稀土及钼、钴含量的X射线荧光光谱测定方法的研究. 高萍等。.光谱学与光谱分析，第23卷第3期. 2003 * |
| 电子计算机在炼油催化剂的X射线荧光光谱分析中的应用. 顾若晶等.石油学报，第2卷第1期. 1986 |
| 电子计算机在炼油催化剂的X射线荧光光谱分析中的应用. 顾若晶等.石油学报，第2卷第1期. 1986 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8880356B2 (en) | 2008-02-06 | 2014-11-04 | Fei Company | Method and system for spectrum data analysis |
| US8664595B2 (en) | 2012-06-28 | 2014-03-04 | Fei Company | Cluster analysis of unknowns in SEM-EDS dataset |
| US9188555B2 (en) | 2012-07-30 | 2015-11-17 | Fei Company | Automated EDS standards calibration |
| US8937282B2 (en) | 2012-10-26 | 2015-01-20 | Fei Company | Mineral identification using mineral definitions including variability |
| US9048067B2 (en) | 2012-10-26 | 2015-06-02 | Fei Company | Mineral identification using sequential decomposition into elements from mineral definitions |
| US9091635B2 (en) | 2012-10-26 | 2015-07-28 | Fei Company | Mineral identification using mineral definitions having compositional ranges |
| US9778215B2 (en) | 2012-10-26 | 2017-10-03 | Fei Company | Automated mineral classification |
| US9194829B2 (en) | 2012-12-28 | 2015-11-24 | Fei Company | Process for performing automated mineralogy |
| US9714908B2 (en) | 2013-11-06 | 2017-07-25 | Fei Company | Sub-pixel analysis and display of fine grained mineral samples |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1601261A (en) | 2005-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100498309C (en) | Method for analyzing metal content in catalytic cracking catalyst through X ray fluorescence method | |
| CN101799437B (en) | Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method | |
| Danyushevsky et al. | Routine quantitative multi-element analysis of sulphide minerals by laser ablation ICP-MS: Standard development and consideration of matrix effects | |
| US9362096B2 (en) | Combustion pretreatment-isotope dilution mass spectrometry | |
| CN103412034A (en) | Measuring method for quickly measuring contents of heavy metals in tobacco by using microwave digestion/ICP-MS method | |
| CN102495042B (en) | Raman spectrum accurate quantitative analysis method of powder mixture | |
| Beary et al. | Development of high-accuracy ICP mass spectrometric procedures for the quantification of Pt, Pd, Rh, and Pb in used auto catalysts | |
| Laserna et al. | Mixture analysis and quantitative determination of nitrogen-containing organic molecules by surface-enhanced Raman spectrometry | |
| CN110514643A (en) | A kind of method that inductively coupled plasma emission spectrography measures trace element in high purity magnesium base oxide | |
| CN105717151B (en) | The measuring method of platinum, samarium element in reforming catalyst | |
| Wang et al. | Simultaneous quantitative analysis of arsenic, bismuth, selenium, and tellurium in soil samples using multi-channel hydride-generation atomic fluorescence spectrometry | |
| Sengupta et al. | Determination of trace elements in carbon steel by inductively coupled plasma atomic emission spectrometry | |
| CN1156690C (en) | Method for determining content of Pt, Eu and Ce elements in reformed catalyst | |
| CN108645687A (en) | A kind of solid organic fertilizer method for detecting element and application | |
| Barshick et al. | Analysis of solution residues by glow discharge mass spectrometry | |
| CN104931575A (en) | Analysis method for identifying gold, platinum and palladium in chemical sample | |
| CN108872283A (en) | Using the method for wavelength dispersion X-ray fluorescence spectrometer measurement plant sample | |
| Śliwiński et al. | Making low concentration in-house pressed pellet trace element standards for carbonate rock analyses by WD-XRF | |
| Kunimura et al. | Application of a portable TXRF spectrometer to determine trace amounts of toxic elements | |
| JP2000074858A (en) | Method for quantitating palladium palladium catalyst | |
| Joshi et al. | Compositional characterization of hafnium recovered from zirconium purification process using total reflection X-ray fluorescence | |
| CN110003247A (en) | A kind of thiophenedicarboxylic acid complex and the preparation method and application thereof | |
| Zolotov | Hybrid methods of analysis. Plenary lecture | |
| Natarajan et al. | Determination of metallic impurities in U3O8 using energy dispersive X-ray fluorescence spectrometry | |
| Wybenga et al. | Determination of Certain Noble Metals in Solution by Means of X-ray Fluorescence Spectroscopy. 2. Determination of Palladium, Rhodium, and Ruthenium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20090610 |
|
| CX01 | Expiry of patent term |