CN106959228A - The processing method of spectrofluorimetry sample - Google Patents
The processing method of spectrofluorimetry sample Download PDFInfo
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- CN106959228A CN106959228A CN201710108087.8A CN201710108087A CN106959228A CN 106959228 A CN106959228 A CN 106959228A CN 201710108087 A CN201710108087 A CN 201710108087A CN 106959228 A CN106959228 A CN 106959228A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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Abstract
The present invention relates to a kind of processing method of spectrofluorimetry sample, including following operation：Sample solution is provided；The sample solution and organic solvent are mixed to get mixed solution, wherein, the boiling point of the organic solvent is more than 150 DEG C, and the organic solvent is miscible with water；And the mixed solution is transferred on carrier, spectrofluorimetry sample is obtained after drying, the carrier is filter paper or inorganic filter membrane.The processing method of above-mentioned spectrofluorimetry sample, the organic solvent with boiling point higher than 150 DEG C is mixed with sample solution, and using filter paper or inorganic filter membrane as carrier, appropriate mixed solution is transferred on carrier.Because the boiling point of the organic solvent is high and water-miscible, thus dry after carrier, organic solvent and the sample being evenly distributed are left on carrier, so as to ensure that the uniformity of sample, measurement accuracy and the degree of accuracy is improved.
Description
Technical field
The present invention relates to analysis and testing technology field, more particularly to a kind of processing method of spectrofluorimetry sample.
Background technology
X-ray fluorescence spectra analysis is a kind of modern instrumental analysis method, with analyze speed is fast, detection range is wide, knot
Really reliable and stable the advantages of.Because X-ray fluorescence spectra analysis is a kind of comparative analysis, the test result of test sample will be with mark
Drawn after quasi- sample, therefore, standard sample and test sample must all have same pattern.Traditional sample treatment side
Method, predominantly powder pressing method.Powder pressing method low cost, it is simple to operate, quick, but the thing phase and granularity of test sample with
When standard sample is inconsistent, serious interference can be produced, causes measurement accuracy and the degree of accuracy poor.
The content of the invention
Based on this, it is necessary to improve the problem of for measurement accuracy after sample treatment and the poor degree of accuracy and survey there is provided one kind
The processing method of accuracy of measurement and the spectrofluorimetry sample of the degree of accuracy.
A kind of processing method of spectrofluorimetry sample, including following operation：
Sample solution is provided；
The sample solution and organic solvent are mixed to get mixed solution, wherein, the boiling point of the organic solvent is more than
150 DEG C, the organic solvent is miscible with water；And
The mixed solution is transferred on carrier, spectrofluorimetry sample is obtained after drying, the carrier is filter paper
Piece or inorganic filter membrane.
In wherein one embodiment, the sample solution is obtained by operating as follows：Acid leach solution sample is used, is obtained
To the sample solution, wherein, the solute of the acid solution in hydrochloric acid, nitric acid, hydrofluoric acid and hydrogen peroxide at least
It is a kind of.
In wherein one embodiment, the concentration of sample is 5g/L~40g/L in the sample solution.
In wherein one embodiment, the operation that the mixed solution is transferred on carrier is：By 50 μ L~500
Mixed solution described in μ L is added dropwise on the carrier.
Described that the mixed solution is transferred in the operation on carrier in wherein one embodiment, the mixing is molten
Liquid is transferred to the center of the carrier.
In wherein one embodiment, the organic solvent is glycerine, propane diols or ethylene glycol.
In wherein one embodiment, the operation that the sample solution and organic solvent are mixed to get to mixed solution
In, the mass ratio that the sample solution is mixed with the organic solvent is 1：0.5~4.
In wherein one embodiment, the spectrofluorimetry sample is analyzed available for X-ray fluorescence spectra.
In wherein one embodiment, in the operation that spectrofluorimetry sample is obtained after the drying, the drying
Temperature is 100 DEG C~150 DEG C.
In wherein one embodiment, the operation that the mixed solution is transferred on carrier is：By the carrier
Be placed in substrate, then the mixed solution be transferred on the carrier, wherein, the substrate be polytetrafluoroethylene (PTFE) substrate or
Person's substrate of glass.
The processing method of above-mentioned spectrofluorimetry sample, is mixed with organic solvent of the boiling point higher than 150 DEG C and sample solution
Close, using filter paper or inorganic filter membrane as carrier, appropriate mixed solution is transferred on carrier.Due to the boiling of the organic solvent
Point is high and water-miscible, thus dries after carrier, organic solvent and the sample being evenly distributed is left on carrier, so as to ensure
The uniformity of sample, improves measurement accuracy and the degree of accuracy.
Brief description of the drawings
Fig. 1 is the flow chart of the processing method of the spectrofluorimetry sample of an embodiment.
Embodiment
It is below in conjunction with the accompanying drawings and specific real to enable the above objects, features and advantages of the present invention more obvious understandable
Example is applied to be described in detail the embodiment of the present invention.Elaborate in the following description many details in order to
Fully understand the present invention.But the invention can be embodied in many other ways as described herein, art technology
Personnel can do similar improvement in the case of without prejudice to intension of the present invention, therefore the present invention is not by following public specific implementation
Limitation.
The processing method of the spectrofluorimetry sample of an embodiment as shown in Figure 1, including following operation.
There is provided sample solution by S110.
Sample solution can be the sample solution prepared or be prepared with solid sample.Sample is molten
The preparation method of liquid is：Acid leach solution sample is used, sample solution is obtained.If necessary, sample solution can be put into constant temperature
In case, High-temperature Digestion sample is carried out.Furthermore, it is possible to which according to test needs, constant volume is carried out to sample solution using water.Sample solution
In, the concentration of sample is 5g/L~40g/L.It is preferred that, the concentration of sample is 20g/L.
Acid solution is generally boiling point below 150 DEG C and volatile solution, or labile solution.It is preferred that,
The solute of acid solution is at least one in hydrochloric acid, nitric acid, hydrofluoric acid and hydrogen peroxide.
Sample in sample solution, can be test sample or standard sample.According to test needs, standard sample
Product answer operation repetitive with test sample.
S120, the sample solution that S110 is obtained is well mixed with organic solvent, mixed solution is obtained, wherein, You Jirong
The boiling point of agent is more than 150 DEG C, and organic solvent is miscible with water.
Organic solvent miscible with water, when being mixed with sample solution, organic solvent can be mixed with sample solution
It is even, obtain uniform mixed solution.After mixed solution is transferred to carrier, the acid solution in sample solution is gone, sample energy
Enough it is evenly distributed in organic solvent so that the thing phase and homogeneous grain diameter of sample.
The boiling point of organic solvent is more than 150 DEG C, and in the step of subsequently removing acid flux material, temperature setting is between acidity
Between the boiling point of solution and the boiling point of organic solvent, then it can will not remove organic solvent while acid solution is removed, make
Organic solvent and equally distributed sample can be stayed on carrier.This both maintains sample homogeneity, and acid solution is eliminated again,
Instrument component is protected in test process.
Wherein, organic solvent is glycerine, propane diols or ethylene glycol.It is preferred that, it is used as organic solvent with glycerine.
The mass ratio of the mixing of sample solution and organic solvent is 1：0.5~4.The mixing of sample solution and organic solvent
The main characteristic according to acid solution and organic solvent of mass ratio and situation about mixing are determined.It is preferred that, sample solution and have
The mass ratio of the mixing of machine solvent is 1：1.
In S120, carrier can be placed in substrate, then mixed solution is transferred on carrier.Substrate is usually cylinder
Body, can be PTFE base bottom or substrate of glass, the standard of selection is that the acid solution used can not occur with substrate
Reaction.Ptfe substrate is used under normal circumstances, is that be can apply to because of the substrate in various acid solutions, and glass base
Plate can react with hydrofluoric acid, using when be subject to certain restrictions.
The size of substrate is determined according to tester.The substrate used in present embodiment is a diameter of 32mm, is highly
10mm cylinder substrate.Filter paper is a diameter of 22mm circular filter paper.
S130, the mixed solution that S120 is obtained is transferred on carrier, and spectrofluorimetry sample is obtained after drying.
By on example enrichment to carrier, wherein, carrier is mainly filter paper or inorganic filter membrane.Filter paper and inorganic filter membrane
Can be qualitatively or quantitative, and filter paper and inorganic filter membrane can be for the filter papers in any aperture and without machine filter
Film.
It is preferred that, inorganic filter membrane can be acetate fiber filter membrane (aperture is preferably 0.45 μm), nylon micro porous filter membrane (aperture
Preferably 0.45 μm), etc..
It is preferred that, the μ L mixed solutions of 50 μ L~500 are pipetted with pipettor, are added dropwise on carrier.Pipette the body of mixed solution
Product is mainly determined by the RSD values and maximum response of response, specifically with the RSD minimums and sound of analog value during sample test
Maximum should be worth to be preferred.The general volume for pipetting mixed solution is 100 μ L.Moreover, mixed solution is typically added dropwise at the center of carrier
Place.So, mixed solution to surrounding extend when, will not be influenceed by edge, it is ensured that the uniformity of sample.
When drying the carrier for carrying mixed solution, it is placed in baking oven and dries, for volatile acid solution, dries
Temperature is less than the boiling point of organic solvent and more than the boiling point of acid solution；For labile acid solution, dry temperature is small
In the boiling point and the temperature acutely decomposed more than acid solution of organic solvent；Usually 100 DEG C~150 DEG C.When acid solution
Solute contains nitric acid, and when organic solvent is glycerine, nitric acid can react with glycerine, generates nitroglycerine, works as temperature
Reach after its demolition point, i.e., can produce blast, so now temperature should be controlled below 170 DEG C.Dry purpose is to remove
Acid solution on carrier, only retains organic solvent and sample so that sample equably can be enriched on carrier, and is prevented
Damage of the acid solution to instrument component.
After high temperature drying, it is necessary to which the carrier for being loaded with sample is cooled into room temperature.Because the organic solvent used holds
Moisture in easy absorption air, thus during cooling, place it in drier.Detection of the moisture to sample can produce certain
Influence, but if when little to detection precision requirement, can also be cooled down without using drier.
The spectrofluorimetry sample that S130 is obtained is analyzed available for X-ray fluorescence spectra.
The spectrofluorimetry sample that S130 is obtained, the thing phase and homogeneous grain diameter of sample, for X-ray fluorescence spectra point
Analysis, can obtain measurement accuracy and the preferable analysis result of the degree of accuracy.And contrasted with molten sheet method, the operation letter of the above method
It is single, low manufacture cost.The operation of acid solution is removed due to being related in method, therefore solves the acid that sample segment is introduced when clearing up
Property material damage instrument the problem of.
The processing method of above-mentioned spectrofluorimetry sample, is mixed with organic solvent of the boiling point higher than 150 DEG C and sample solution
Close, using filter paper or inorganic filter membrane as carrier, appropriate mixed solution is transferred on carrier.Due to the boiling of the organic solvent
Point is high and water-miscible, thus dries after carrier, organic solvent and the sample being evenly distributed is left on carrier, so as to ensure
The uniformity of sample, improves measurement accuracy and the degree of accuracy.
Embodiment 1
0.5000g nickel copper zinc ferrite powders are weighed in the high pressure solution bullet tanks of 50mL, 10mL 36wt% hydrochloric acid is added,
It is put into thermostatic drying chamber, from room temperature to constant temperature 1h after 180 DEG C.Taken out after cooling, solution is transferred in 25mL volumetric flasks,
Scale is diluted with water to, mixes, sample solution is made.
1.000g glycerine and 1.000g sample solution are weighed respectively, mix, mixed solution is made.
A diameter of 22mm filter paper is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
100 μ L mixed solution is pipetted using micropipettor, mixed solution is dropped in into filter paper center.
The substrate for being placed with filter paper is put into baking oven, is heated to from room temperature after 150 DEG C, constant temperature 30min.
After 30min, it is drawn off being placed in drier and is cooled to room temperature.
Standard sample preparation method is consistent with sample powder preparation method.
Embodiment 2
There is provided containing nitric acid, hydrofluoric acid, zirconium, yttrium, hafnium element acid heavy metal solution.
1.000g glycerine and 1.000g sample solution are weighed respectively, mix, mixed solution is made.
A diameter of 22mm filter paper is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
100 μ L mixed solution is pipetted using micropipettor, mixed solution is dropped in into filter paper center.
The substrate for being placed with filter paper is put into baking oven, 150 DEG C are heated to from room temperature, 30min is incubated.
After 30min, it is drawn off being placed in drier and is cooled to room temperature.
Standard sample preparation method is consistent with sample powder preparation method.
Embodiment 3
0.5000g silver pastes are weighed in 250mL glass beakers, 10mL 68wt% nitric acid is slowly added to, question response stops
Afterwards, it is positioned on electric hot plate and is heated to solution without significant change.Taken out after cooling, solution is transferred in 25mL volumetric flasks, uses water
Scale is diluted to, mixes, sample solution is made.
1.000g propane diols and 2.000g sample solution are weighed respectively, mix, mixed solution is made.
A diameter of 22mm filter paper is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
100 μ L mixed solution is pipetted using micropipettor, mixed solution is dropped in into filter paper center.
The substrate for being placed with filter paper is put into baking oven, is heated to from room temperature after 150 DEG C, constant temperature 30min.
After 30min, it is drawn off being placed in drier and is cooled to room temperature.
Standard sample preparation method is consistent with sample powder preparation method.
Embodiment 4
0.1250g nickel copper zinc ferrite powders are weighed in the high pressure solution bullet tanks of 50mL, the hydrochloric acid that 6mL contains 36wt% is added
With the mixed acid solution of 1mL 40wt% hydrofluoric acid, it is put into thermostatic drying chamber, from room temperature to constant temperature after 180 DEG C
1h.Taken out after cooling, solution is transferred in 25mL volumetric flasks, is diluted with water to scale, mix, sample solution is made.
0.500g ethylene glycol and 1.000g sample solution are weighed respectively, mix, mixed solution is made.
A diameter of 22mm inorganic filter membrane is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
500 μ L mixed solution is pipetted using micropipettor, mixed solution is dropped in into filter paper center.
The substrate for being placed with filter paper is put into baking oven, is heated to from room temperature after 100 DEG C, constant temperature 45min.
After 45min, it is drawn off being placed in drier and is cooled to room temperature.
Standard sample preparation method is consistent with sample powder preparation method.
Embodiment 5
1.0000g nickel copper zinc ferrite powders are weighed in the high pressure solution bullet tanks of 50mL, the salt that 5mL contains 36wt% is added
The hydrogen peroxide of acid, 2mL 68wt% nitric acid and 1mL 40wt%, is put into thermostatic drying chamber, from room temperature to 180 DEG C
Constant temperature 1h afterwards.Taken out after cooling, solution is transferred in 25mL volumetric flasks, is diluted with water to scale, mix, sample solution is made.
4.000g ethylene glycol and 1.000g sample solution are weighed respectively, mix, mixed solution is made.
A diameter of 22mm inorganic filter membrane is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
50 μ L mixed solution is pipetted using micropipettor, mixed solution is dropped in into filter paper center.
The substrate for being placed with filter paper is put into baking oven, is heated to from room temperature after 125 DEG C, constant temperature 25min.
After 25min, it is drawn off being placed in drier and is cooled to room temperature.
Standard sample preparation method is consistent with sample powder preparation method.
Embodiment 6
The preparation of standard sample：
According to the form below 1 weighs mangano-manganic oxide, zinc oxide, iron oxide high purity material in 5 high pressure solution bullet tank.
Table 1：The raw material composition of standard items
| Weigh | Mn3O4 | Fe2O3 | ZnO |
| 1 | 0.125g | 0.250g | 0.125g |
| 2 | 0.100g | 0.300g | 0.100g |
| 3 | 0.080g | 0.345g | 0.075g |
| 4 | 0.065g | 0.375g | 0.060g |
| 5 | 0.050g | 0.400g | 0.050g |
10mL 36wt% hydrochloric acid is added, is put into thermostatic drying chamber, from room temperature to constant temperature 1h after 180 DEG C.Cooling
After take out, solution is transferred in 25mL volumetric flasks, is diluted with water to scale, mix, standard items material solution is made.
1.000g glycerine and 1.000g standard solution are weighed respectively, mix, standard items raw material mixed solution is made.
A diameter of 22mm filter paper is placed in a diameter of 32mm, a height of 10mm polytetrafluoroethylene (PTFE) column base.
100 μ L standard items raw material mixed solution is pipetted using micropipettor, standard items raw material mixed solution is dropped in
Filter paper center.
The substrate for being placed with filter paper is put into baking oven, is heated to from room temperature after 150 DEG C, constant temperature 30min.
After 30min, it is drawn off being placed in drier and is cooled to room temperature, obtains standard items.
The preparation of sample：
Two parts of 0.5000g manganese-zinc ferrite powders are weighed, in 2 high pressure solution bullet tank, preparation method and standard sample system
Preparation Method is consistent.
The standard sample prepared is put into Xray fluorescence spectrometer, standard sample entered according to instrument optimum condition
Row analysis, using target oxide response as ordinate, target oxide proportion is abscissa, draws standard curve.
Sample is analyzed with the same terms, show that sample analysis result is as shown in table 2 below.
Table 2：The test result of sample
| Target compound | Mn3O4 | Fe2O3 | ZnO |
| Test value 1 | 16.49% | 68.62% | 14.93% |
| Test value 2 | 16.70% | 68.58% | 14.66% |
| Average value | 16.59% | 68.60% | 14.80% |
| Reference value | 16.62% | 68.47% | 14.91% |
| Deviation | - 0.03% | 0.13% | - 0.11% |
Reference value is drawn by chemical method analysis.
As can be seen from Table 2, the deviation of the test result of sample is low, this method of testing measurement accuracy and the degree of accuracy compared with
It is high.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of processing method of spectrofluorimetry sample, it is characterised in that including following operation：
Sample solution is provided；
The sample solution and organic solvent are mixed to get mixed solution, wherein, the boiling point of the organic solvent is more than 150 DEG C
And it is miscible with water；And
The mixed solution is transferred on carrier, spectrofluorimetry sample is obtained after drying, the carrier be filter paper or
Inorganic filter membrane.
2. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that the sample solution leads to
Following operation is crossed to be made：Acid leach solution sample is used, the sample solution is obtained, wherein, the solute choosing of the acid solution
At least one from hydrochloric acid, nitric acid, hydrofluoric acid and hydrogen peroxide.
3. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that in the sample solution
The concentration of sample is 5g/L~40g/L.
4. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that described by the mixing
The operation that solution is transferred on carrier is：Mixed solution described in the μ L of 50 μ L~500 is added dropwise on the carrier.
5. the processing method of the spectrofluorimetry sample according to claim 1 or 4, it is characterised in that described by described in
Mixed solution is transferred in the operation on carrier, and the mixed solution is transferred to the center of the carrier.
6. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that the organic solvent is
Glycerine, propane diols or ethylene glycol.
7. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that described by the sample
Solution is mixed to get in the operation of mixed solution with organic solvent, the mass ratio that the sample solution is mixed with the organic solvent
For 1：0.5~4.
8. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that the fluorescence spectrum point
Sample is analysed to analyze available for X-ray fluorescence spectra.
9. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that obtained after the drying
In the operation of spectrofluorimetry sample, the temperature of the drying is 100 DEG C~150 DEG C.
10. the processing method of spectrofluorimetry sample according to claim 1, it is characterised in that described described to mix
Closing the operation that is transferred on carrier of solution is：The carrier is placed in substrate, then the mixed solution is transferred to described
On carrier, wherein, the substrate is polytetrafluoroethylene (PTFE) substrate or substrate of glass.
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| CN113607763A (en) * | 2021-07-30 | 2021-11-05 | 苏州西热节能环保技术有限公司 | Component analysis sample preparation method and device for flat-plate catalyst |
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| CN106959228B (en) | 2020-03-17 |
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