CN1249425A - Sample preparation method for X-ray spectral analysis - Google Patents
Sample preparation method for X-ray spectral analysis Download PDFInfo
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- CN1249425A CN1249425A CN 99111593 CN99111593A CN1249425A CN 1249425 A CN1249425 A CN 1249425A CN 99111593 CN99111593 CN 99111593 CN 99111593 A CN99111593 A CN 99111593A CN 1249425 A CN1249425 A CN 1249425A
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Abstract
A sample preparation method for X-ray spectral analysis is used for preparing test samples such as minerals for analysis by X-ray fluorescence spectrometry. The method is characterized in that elements to be detected in a sample are converted into meltable salts, a mixed solution of citric acid (sodium) and E DTA is added, the concentration of the citric acid (sodium) in the solution is 15 g/l-25 g/l, the concentration of EDTA is 6 g/l-10 g/l, the pH value of the solution is 4-9, and agarose is added to prepare a gel solid sample. The element is distributed evenly, no granularity effect is generated, no leakage is generated, the operation method is simple, the sample can be stored for a long time, and the method has the advantages of a solution method and a solid method, and is an ideal sample preparation method for X-ray spectral analysis.
Description
The method for making sample that is used for X-ray spectral analysis, when relating to a kind of component that adopts samples such as x ray fluorescence spectrometry assaying, the method for preparation standard sample and specimen.
When carrying out X-ray spectral analysis, require analytic sample to have smooth surface, element is evenly distributed.During analysis, need preparation corresponding standard sample, and standard model to be consistent with the physical form of sample, to guarantee the reliability of analysis result.The preparation sample is the important step of carrying out X-ray spectral analysis.At present, carrying out the sample preparation methods that X-ray spectral analysis mainly adopts both at home and abroad has following several: (1) alloy block sample method.Be about to metal and alloy and make the piece sample, polishing is carried out on its surface made.(2) powder pressing method.Be mainly used in sample analysis such as ore, rock, soil, cement, pottery, slag, sediment.Said method, grind away polishing process trouble, time-consuming, and powder pressing method is difficult to eliminate fully granularity effect and heterogeneous effect.(3) fusion method.Powdered sample is mixed with flux (as sodium tetraborate, lithium tetraborate or lithium metaborate etc.), and the vitreum sheet is made in fusing in golden platinum pincers crucible.The main preparation of using the specimen of ore, rock etc.(4) liquid and solwution method are to make solution after the process chemical treatments such as ore, to place sample cell.Liquid processes and solwution method have its unique advantage, and element distributes very evenly, and can eliminate the granularity effect fully, operate also fairly simple, quick.But adopt liquid and solwution method, leak of liquid takes place easily, instrument is produced harmful effect, and standard specimen and sample all are difficult to long preservation.
Purpose of the present invention is exactly the deficiency that exists in the above-mentioned prior art in order to overcome, and provides a kind of element to be evenly distributed, and no granularity effect does not produce leakage, simple, the sample a kind of method for making sample that is used for X-ray spectral analysis with long preservation period of method of operating.
The objective of the invention is to be achieved through the following technical solutions.
The method for making sample that is used for X-ray spectral analysis, preparation process comprises that analytical sample decomposes, wherein element to be measured converts the meltability salt to, it is characterized in that: a. is to changing the sample to be tested that changes into the meltability salt, add the mixed solution of citric acid (sodium) and EDTA, make sample solution, citric acid in the solution (sodium) concentration is 15g/l-25g/l, EDTA concentration concentration 6g/l-10g/l, the pH value of solution is 4-9; B. add agarose in solution, be heated to 85 ℃-95 ℃, make in the solution agarose dissolving make colloidal sol, be cooled to gel solid shape print then, the addition of its agarose is 15g/l-30g/l.
Adopt method for making sample of the present invention, when liquid sample analysis is carried out specimen preparation, at first solution is carried out heating evaporation, add the mixed solution of citric acid (sodium) and EDTA again, make test solution, in solution, add agarose and make to doing.
Adopting method for making sample of the present invention, when liquid sample analysis is prepared sample, is the mixed solution that directly adds citric acid (sodium) and EDTA at solution, makes test solution, adds agarose and make in solution.
Method of the present invention adds in sample solution and has strong citric acid of comprehensive complexing power (sodium) and EDTA mixed twine mixture, regulate certain pH value, make metallic ion to be measured in the solution under the effect of comprehensive complexing agent, being the complex compound form is evenly distributed in the solution, add gelatinous mass, heating makes gelatinous mass be dispersed into colloidal sol in sample solution, metallic ion to be measured in the colloidal sol is evenly distributed, overcome the element compound precipitation that exists in the prior art effectively, the composition skewness that produces, and granularity is imitated the harmful effect that produces.Cooling back glue promptly forms gel, thereby makes solid shape print, is used for X-ray spectral analysis, has eliminated prior art test sample preparation difficulty effectively, and may produce the shortcoming of leakage, and sample is easy to preserve.
The gelatinous mass agarose that the present invention uses can evenly disperse the formation glue when temperature is higher than 80 ℃, and glue is cooled to 35 ℃ in aqueous solution, and the concentration that needs only glue reaches 5g/l when above, can form gel.When the concentration of the aqueous dispersions of agarose was equal to or greater than 15g/l, the gelatinous mass that can form was highly stable, elasticity slightly, and its suitable pH value scope is 4-9.But in the pH value is the 4-9 scope, because many heavy metal ion might form precipitation, method of the present invention for this reason, adopt the method for the mixed twine mixture that adds citric acid (sodium) and EDTA composition, heavy metal ion can be remained in the solution effectively, heavy metal ion is evenly distributed effectively, for the constituent content of accurately testing in the sample ore provides assurance in the gel of preparation.
The X-ray spectral analysis sample of method preparation of the present invention, its element is evenly distributed, no granularity effect, but do not produce leakage, simple, the print long preservation of method of operating, the advantage of existing solwution method has the advantage of solid process again, is a kind of method for making sample of very desirable X-ray spectral analysis.
Below in conjunction with example method of the present invention is described further.
The method for making sample that is used for X-ray spectral analysis, at first analytical sample is decomposed, wherein element to be measured converts the solubility salt to conventional method, with this solubility salt, add the mixed solution of citric acid (sodium) and EDTA, make sample solution, wherein citric acid (sodium) concentration is 15g/l-25g/l, EDTA concentration concentration 6g/l-10g/l, the pH value of solution is 4-9; Add agarose then in solution, be heated to 85 ℃-95 ℃, make in the solution agarose dissolving make colloidal sol, be cooled to gel solid shape print, the addition of agarose is 15g/l-30g/l.
Embodiment 1
Measure lead, zinc, iron content in the plumbous zinc ore.
(1) standard solution preparation
At first preparing standard solution is prepared lead, iron, each 10mg/ml of zinc mother liquor (plumbous mother liquor is a nitric acid medium, and zinc, iron mother liquor are hydrochloric acid medium) respectively.
(2) standard specimen preparation
Get 7 mixed standard solutions of respective standard mother liquor preparation, each element mass concentration scope is as follows:
Pb：??0.1-3.5g/l；
Zn：??0.1-3.0g/l；
Fe：??0.3-1.5g/l；
Get 20ml and mix mark mark solution in the 50ml beaker, heating adds 20g/l citric acid-8g/lEDTA mixed solution 20ml after closely doing, the low-grade fever dissolving, add the 0.3g agarose, be heated to 90 ℃, shake up dissolving after, the sol solutions that makes moves into sample cell, and cooled and solidified is made standard model.
(3) specimen preparation
Take by weighing the 0.25g sample ore, add 10ml hydrochloric acid, heating for dissolving is driven away sulfuretted hydrogen, adds 5ml nitric acid, continue to be heated to dissolving fully after, be evaporated to dried.Add 8 of hydrochloric acid (1+1) again, moistening salt also makes oxygenate conversion become soluble salt, the mixed solution 20ml that adds 50g/l citric acid and 20g/l EDTA again, heating makes the salt dissolving, the cooling back is settled to 50ml (about pH value=5) with water, pipette 20ml and add the 0.3g agarose, operation prepares with standard specimen below.
(4) test
Adopt Xray fluorescence spectrometer, measure the PbL in the standard specimen
β 1, ZnK
α, FeK
αThe fluorescence intensity of analytical line, the drawing curve.Measure the intensity of each element in the sample under the same conditions, according to the content of Pb, Zn, Fe in the corresponding work curve calculation sample.
Adopt method income analysis result of the present invention and chemical method to record result's contrast, see Table 1.
Table 1
| Sample number into spectrum | Element | This law analysis result, % | The chemical method result, % | |
| Measure | On average | |||
| The 1# sample ore | ????Pb | ??36.67，36.52，36.69，36.54 | ????36.61 | ????36.85 |
| ????Zn | ??7.41，7.39，7.49，7.45 | ????7.44 | ????7.40 | |
| ????Fe | ??19.15，19.35，19.45，19.60 | ????19.39 | ????19.59 | |
| The 2# sample ore | ????Pb | ??8.62，8.63，8.79 | ????8.68 | ????8.65 |
| ????Zn | ??53.80，53.85，53.60 | ????53.75 | ????53.60 | |
| ????Fe | ??8.20，8.15，8.25 | ????8.20 | ????8.30 | |
Experiment shows that this method is simple to operate, and precision is good, and sample can be preserved and not go bad in 3 months, and is easy to use.
Embodiment 2
Measure copper, iron content in the solution.
Getting the neutral indicator of neutral indicator (1g/l) 0.1g is dissolved in 100ml 60% ethanol.
(1) standard solution preparation
Prepare 10mg/ml copper, iron, zinc mother liquor (the copper mother liquor is a nitric acid medium, and the iron mother liquor is a hydrochloric acid medium) respectively.
(2) standard specimen preparation
Get 7 mixed standard solutions of respective standard mother liquor preparation, each element mass concentration scope is as follows:
Cu：??0.2g/l-3g/l；
Fe：??0.6g/l-4.0g/l；
Get 20ml and mix mark mark solution in the 50ml volumetric flask, add 50g/l citric acid-20g/lEDTA mixed solution 20ml, add 1 of the neutral indicator of 1g/l, regulate pH value to solution with ammoniacal liquor (1+3) and hydrochloric acid (1+3) and redden (pH=6.5), with the water constant volume.Pipette 20ml solution and place the beaker of 50ml, add the 0.3g agarose, be heated to 90 ℃, shake up dissolving after, the sol solutions that makes is moved into sample cell, cooled and solidified is made standard model and is preserved.
(3) specimen preparation
Get the 20ml test solution in the volumetric flask of 50ml, below operation prepares with standard specimen.
(4) test
Adopt Xray fluorescence spectrometer, measure the CuK in the standard specimen
α, FeK
αThe fluorescence intensity of analytical line, the drawing curve.Measure the intensity of each element in the sample under the same conditions, according to the content of Cu, Fe in the corresponding work curve calculation sample.
With method of the present invention copper in the solution, iron content are carried out 7 times and measure, income analysis result and solution-X-ray fluorescence spectra analytic approach gained result contrast sees Table 2.
Table 2 method of the present invention and solution-xrf method analysis result contrast
| Element | This law analysis result, g/L | Solution-XRF method, g/L | ||
| Measured value | Mean value | Standard deviation | ||
| ??Cu | ?1.203，1.196，1.200，1.204，1.205， ?1.203，1.204 | ?1.202 | ?0.0031 | ?1.200 |
| ??Fe | ?0.866，0.864，0.863，0.868，0.861， ?0.867，0.866 | ?0.865 | ?0.0024 | ?0.870 |
Experimental result shows, the accuracy height of its method fully can be as the ultimate analysis in mineral and the various solution, and its method is easy to be reliable.
Claims (3)
1. the method for making sample that is used for X-ray spectral analysis, preparation process comprise that analytic sample decomposes, and wherein element to be measured converts the meltability salt to, it is characterized in that:
A. to changing the sample to be tested that changes into the meltability salt, add the mixed solution of citric acid (sodium) and EDTA, make sample solution, citric acid in the solution (sodium) concentration is 15g/l-25g/l, and EDTA concentration concentration is 6g/l-10g/l, and the pH value of solution is 4-9;
B. add agarose in solution, be heated to 85 ℃-95 ℃, make the agarose dissolving make colloidal sol, be cooled to gel solid shape print, the addition of its agarose is 15g/l-30g/l.
2. method according to claim 1, it is characterized in that: at the specimen preparation that carries out liquid sample analysis, be that solution is carried out heating evaporation to doing, add the mixed solution of citric acid (sodium) and EDTA again, make test solution, in solution, add agarose and make.
3. method according to claim 1 is characterized in that: at the specimen preparation that carries out liquid sample analysis, be the mixed solution that directly adds citric acid (sodium) and EDTA at solution, make test solution, add agarose and make in solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99111593 CN1094590C (en) | 1999-08-20 | 1999-08-20 | Sample preparation method for X-ray spectral analysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99111593 CN1094590C (en) | 1999-08-20 | 1999-08-20 | Sample preparation method for X-ray spectral analysis |
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| CN1249425A true CN1249425A (en) | 2000-04-05 |
| CN1094590C CN1094590C (en) | 2002-11-20 |
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| CN 99111593 Expired - Fee Related CN1094590C (en) | 1999-08-20 | 1999-08-20 | Sample preparation method for X-ray spectral analysis |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101368887B (en) * | 2008-09-13 | 2011-05-25 | 中国科学院青海盐湖研究所 | Gel sampling method of oil-field water and bittern used for X-ray fluorescence spectrum analysis |
| CN101688823B (en) * | 2007-07-24 | 2011-09-14 | 乌拉尔卡里技术联合股份有限公司 | Method for preparing samples for quantitatively and qualitatively determining the precious metal content in products of processing of potassium and magnesium ores |
| CN103207197A (en) * | 2013-03-01 | 2013-07-17 | 中华人民共和国山东出入境检验检疫局 | X-ray fluorescence spectra analysis method for copper content of copper ore |
| CN112067644A (en) * | 2020-08-18 | 2020-12-11 | 铜陵有色金属集团股份有限公司 | Method for detecting liquid sample by adopting X-ray fluorescence spectrometry and sample treatment method |
-
1999
- 1999-08-20 CN CN 99111593 patent/CN1094590C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101688823B (en) * | 2007-07-24 | 2011-09-14 | 乌拉尔卡里技术联合股份有限公司 | Method for preparing samples for quantitatively and qualitatively determining the precious metal content in products of processing of potassium and magnesium ores |
| CN101368887B (en) * | 2008-09-13 | 2011-05-25 | 中国科学院青海盐湖研究所 | Gel sampling method of oil-field water and bittern used for X-ray fluorescence spectrum analysis |
| CN103207197A (en) * | 2013-03-01 | 2013-07-17 | 中华人民共和国山东出入境检验检疫局 | X-ray fluorescence spectra analysis method for copper content of copper ore |
| CN112067644A (en) * | 2020-08-18 | 2020-12-11 | 铜陵有色金属集团股份有限公司 | Method for detecting liquid sample by adopting X-ray fluorescence spectrometry and sample treatment method |
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| Publication number | Publication date |
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| CN1094590C (en) | 2002-11-20 |
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