CN102288460A - Preenrichment sampling method for detecting trace noble metal by X-ray fluorescence - Google Patents
Preenrichment sampling method for detecting trace noble metal by X-ray fluorescence Download PDFInfo
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Abstract
The invention discloses a preenrichment sampling method for detecting a trace noble metal by X-ray fluorescence, which comprises the following steps: first synthesizing beta-cyclodextrin cross-linked resin, and then crushing the beta-cyclodextrin cross-linked resin, sieving the crushed [beta]-cyclodextrin cross-linked resin, adding the screened beta-cyclodextrin cross-linked resin to a prepared standard solution of the noble metal to be detected, adequately oscillating, and then carrying out filtration by using an aqueous microporous filter membrane, so that enriched products are adhered onto the filter membrane and uniformly centralized in a measuring area range of the X-ray fluorescence, baking the products, and finally keeping the products smooth. By using the method provided by the invention, when a noble metal sample is detected by an X-ray fluorescent spectrometry, the problems that the detection limit is higher and the detection of a liquid sample containing the trace metal is difficult to carry out by adopting a conventional sampling method are solved; the method has the advantages of simple equipment, short time consumption, simpleness and convenience in operation, and the like; and the application of an X-ray fluorescence method on the aspect of the detection of the trace metal is broadened.
Description
Technical field
The present invention relates to a kind of preenrichment method for making sample that XRF detects trace noble metal that is used for, belong to materialization detection technique field.
Background technology
Existing report x-ray fluorescence method (XRF) detects the method for noble metal, generally adopts fusion method, directly solid sample is made fuse piece, not only equipment and reagent cost height, and operation requires highly, wastes time and energy.Simultaneously, adopt conventional fusion method, pressed disc method sample preparation to detect noble metal,, limited the application of x-ray fluorescence method in the trace noble metal context of detection because method detects limit for height.Therefore, research is made the method that approaches sample with the noble metal preconcentration, and is significant to the application of x-ray fluorescence method in the analysis of trace noble metal element.
Summary of the invention
The objective of the invention is to remedy the deficiency of above-mentioned prior art, a kind of preenrichment method for making sample that XRF detects trace noble metal that is used for is provided, it is simple to have equipment, weak point consuming time, advantage such as easy and simple to handle has reduced analysis cost and energy consumption, meets energy conservation and environment protection.
For achieving the above object, the technical solution adopted in the present invention is: a kind of preenrichment method for making sample that is used for XRF detection trace noble metal may further comprise the steps at least:
(1) adding the capacity mass percent concentration in the container that fills beta-schardinger dextrin-is 30%～50% sodium hydroxide solution, vibrate in 40 ℃～60 ℃ waters bath with thermostatic control behind the mixing, after the transparent uniform solution to be formed, drip epichlorokydrin to reaction system, the amount ratio of beta-schardinger dextrin-and epichlorokydrin is 1g: 1～3mL, continue concussion, obtain the transparent gel-form product, the product taking-up is smashed to pieces,, behind acetone rinsing, dry again to neutral with distilled water flushing, obtain the beta-schardinger dextrin-cross-linked resin, put in the exsiccator preserve standby;
(2) dried beta-schardinger dextrin-cross-linked resin is pulverized, sieve, ratio in 1g: 0.5L～25L is mixed the beta-schardinger dextrin-cross-linked resin with the standard solution of precious metal element to be measured, the concentration of precious metal ion is 10 μ g/L～1000 μ g/L in the standard solution, fully after the vibration, with water system miillpore filter suction filtration, make enriched product attached to also evenly focusing in the survey area scope of XRF on the water system miillpore filter;
(3) will be attached with the water system miillpore filter tiling back oven dry of enriched product, obtain being used for the preenrichment sample that XRF detects trace noble metal.
The temperature of water bath with thermostatic control is 50 ℃ in the step (1).
Be that dried beta-schardinger dextrin-cross-linked resin is pulverized in the step (2), cross 160～200 mesh sieves.Count in the scope at selected order, resin powder particle diameter small sample configuration of surface more is good more, and the rate of adsorption is fast, and the suction filtration time increases not obvious, does not influence sample preparation efficient.
Fully vibrating in the step (2) is under the water bath with thermostatic control condition, and the temperature of water bath with thermostatic control is 15～40 ℃.
The suction filtration process is filter bowl to be placed carry out suction filtration on the core in the step (2), used filter bowl is made of and both ends open the upper cup and the bottom cup of hollow, the xsect at the arbitrary place of upper cup is circular, cross-sectional diameter from the top end opening of upper cup to the bottom end opening of upper cup reduces gradually, the bottom cup is cylindric, the bottom end opening equal diameters of the top end opening of bottom cup and upper cup, the top end opening of bottom cup are connected with the bottom end opening of upper cup makes upper cup and bottom cup form one.
The edge of the longitudinal section of upper cup is curved.
It is inverted trapezoidal that the longitudinal section of upper cup is.
The area of the xsect of bottom cup is no more than the survey area of XRF.
The bottom end opening of bottom cup is a ground.
Compared with prior art, the present invention has the following advantages:
When preenrichment method for making sample provided by the invention has overcome x ray fluorescence spectrometry detection noble metal sample, adopt conventional method for making sample detection limit fluid sample higher and that be difficult to contain trace-metal to detect problem, have simple, the consuming time weak point of equipment, advantage such as easy and simple to handle, analysis cost and energy consumption have been reduced, meet energy conservation and environment protection, widened the application of x-ray fluorescence method in the trace-metal context of detection.
Description of drawings
Fig. 1 is the infrared spectrum of beta-schardinger dextrin-;
Fig. 2 is the infrared spectrum of the synthetic beta-schardinger dextrin-cross-linked resin of embodiment 1;
Fig. 3 is the one-piece construction synoptic diagram of the used filter bowl of the embodiment of the invention, among the figure, and 1: upper cup; 2: the bottom cup; 3: the top end opening of upper cup; 4: the bottom end opening of bottom cup;
Fig. 4 is the XRF scanning spectrogram of platinum enriched sample among the embodiment 1;
Fig. 5 is the XRF scanning spectrogram of golden enriched sample among the embodiment 1;
Fig. 6 be the synthetic beta-schardinger dextrin-cross-linked resin of embodiment 1 before to the palladium solution absorbs concentration and the comparative result figure of the filter liquor concentration after the absorption;
Fig. 7 detects the canonical plotting of golden enriched sample for XRF.
Embodiment
The present invention is further illustrated below by specific embodiment, but protection content of the present invention is not limited to following examples.
Take by weighing the 5g beta-schardinger dextrin-in the 250mL of tool grinding port plug conical flask, (add that distilled water is wetting to be helped follow-up beta-schardinger dextrin-and mix more even with NaOH with about 3～5mL distilled water is fully wetting, its consumption generally can make beta-schardinger dextrin-fully wetting just passable, also adding distil water not), adding concentration is 12.5moL/L sodium hydroxide solution 6.5mL (the sodium hydroxide solution capacity gets final product), cover the grinding port plug mixing, put into immediately the water bath with thermostatic control oscillator in 50 ℃ with the 200r/min velocity fluctuation, after treating that the beta-schardinger dextrin-dissolving is completed into transparent uniform solution, slowly drip the 6mL epichlorokydrin to reaction system, continue vibration 1 hour, obtain the transparent gel-form lump.Product taken out smashs to pieces, to neutral, use acetone rinsing again 3～5 times,, obtain white or grizzled particle shape beta-schardinger dextrin-cross-linked resin in 70 ℃ of oven dry 12 hours with distilled water flushing, put preserve in the exsiccator stand-by.The infrared spectrum of the beta-schardinger dextrin-cross-linked resin that beta-schardinger dextrin-and present embodiment are synthetic respectively as depicted in figs. 1 and 2.
Among Fig. 2,3415cm
-1The last one absorption peak is arranged, belong to-stretching vibration peak of OH, at 2927cm
-1For-CH
2The flexural vibrations peak, at 1037cm
-1The strong stretching vibration absorption peak of C-O-C has appearred, with among Fig. 1 the reaction before beta-schardinger dextrin-compare, the C-O-C stretching vibration absorption peak of this cross-linking products is wideer, show epichlorokydrin immobilized beta-schardinger dextrin-.
Dried beta-schardinger dextrin-cross-linked resin is pulverized, crossed 200 mesh sieves, the parallel beta-schardinger dextrin-cross-linked resin that takes by weighing after two parts of 0.1g sieve joins in the dry conical flask of two 250mL.Other prepares the goldstandard solution 50mL that platinum standard solution 50mL that platinum ion concentration is 0.8 μ g/mL and gold ion concentration are 0.5 μ g/mL, add respectively in the above-mentioned conical flask, 30 ℃ of vibrations of constant temperature are after 2 hours in the water bath with thermostatic control oscillator, take out with 0.45 μ m water system miillpore filter suction filtration, make enriched product attached to also evenly focusing in the test area scope of XRF detection trace noble metal on the water system miillpore filter.For the product that obtains enrichment can be focused in the needed test area scope more equably, used filter bowl structure as shown in Figure 3 during suction filtration, this filter bowl is by the upper cup 1 of hollow and bottom cup 2 constitutes and both ends open (is illustrated with dotted line among Fig. 3, the above part of dotted line is represented upper cup 1, the following part of dotted line is represented bottom cup 2), the xsect at arbitrary place of upper cup 1 is circular, cross-sectional diameter from the top end opening 3 of upper cup to the bottom end opening of upper cup reduces gradually, the edge of the longitudinal section of present embodiment middle and upper part cup 1 is curved, upper cup 1 the longitudinal section also can be inverted trapezoidal.Bottom cup 2 is cylindric, the bottom end opening equal diameters of the top end opening of bottom cup and upper cup, the top end opening of bottom cup is connected with the bottom end opening of upper cup makes upper cup and bottom cup form one, the cross-sectional area of bottom cup 2 is no more than the survey area of XRF, and the bottom end opening 4 of bottom cup is a ground.The bottom end opening 4 of the bottom cup of above-mentioned filter bowl is lain against core top down get final product suction filtration.Because the cross-sectional diameter of the upper cup of filter bowl reduces gradually, during suction filtration, solution system is cushioned along the flow velocity of filter bowl wall of cup, reduced being enriched in the impulsive force of the sample on the water system miillpore filter, enriched product is focused in the measurement range of XRF more equably, the accuracy that helps testing.
Behind the suction filtration, the filter membrane that is attached with enriched product is taken off, in 60 ℃ of oven dry 4 hours, in drying course, can adopt filter membrane is tiled in method in the double dish that is lined with filter paper, obtain drying the thin sample of enrichment that the back keeps smooth, (purpose of adding a cover preservative film is to prevent from carrying out in the vacuum of XRF detection for the preservative film of 4cm * 4cm in size on its surface cover at last, enriched product comes off from filter membrane and pollutes vacuum chamber), promptly obtain being used for XRF and detect the preenrichment sample, the XRF scanning result of platinum enriched sample and golden enriched sample is distinguished as shown in Figure 4 and Figure 5.
Take by weighing the 10g beta-schardinger dextrin-in the conical flask of tool grinding port plug, after adding 10mL distilled water makes beta-schardinger dextrin-fully wetting, adding concentration is 7.5moL/L sodium hydroxide solution 30mL, cover mixing behind the grinding port plug, put into immediately the water bath with thermostatic control oscillator in 60 ℃ with the 100r/min velocity fluctuation, treat that beta-schardinger dextrin-dissolving is completed into transparent uniform solution after, slowly drip the 15mL epichlorokydrin to reaction system, continue vibration 1.5 hours, obtain the transparent cake product.Smash this product to pieces taking-up, to neutrality, use acetone rinsing again 3 times with distilled water flushing, 60 ℃ of oven dry obtain the white granular product.Adopt the method identical that product is characterized, confirm that this product is the beta-schardinger dextrin-cross-linked resin with embodiment 1.
Get the dried beta-schardinger dextrin-cross-linked resin of an amount of embodiment 1 gained, with its pulverizing, cross 160 mesh sieves, parallelly take by weighing 5 parts of beta-schardinger dextrin-cross-linked resins after sieving, every part of 0.1g joins respectively in the dry conical flasks of 5 250mL.Other prepares each 50mL of palladium standard solution that palladium ion concentration is respectively 20 μ g/L, 50 μ g/L, 100 μ g/L, 200 μ g/L and 300 μ g/L, add respectively in above-mentioned 5 conical flasks, 35 ℃ of following vibrations of constant temperature are after 1 hour in the water bath with thermostatic control oscillator, take out and use filter bowl suction filtration described in 0.45 μ m water system miillpore filter and the embodiment 1 respectively, obtain enriched product.Collect corresponding filtrate respectively, detect filter liquor concentration with graphite furnace atomic absorption spectrophotometer, and the concentration of palladium standard solution before result and the absorption compared, adsorption effect as shown in Figure 6, the concentration of palladium standard solution before a represents to adsorb among the figure, b represents the concentration of beta-schardinger dextrin-cross-linked resin absorption back suction filtration gained filtrate.By Fig. 6 result as can be known, the beta-schardinger dextrin-cross-linked resin has higher adsorption rate to the low concentration palladium.
Get the beta-schardinger dextrin-cross-linked resin after an amount of embodiment 1 gained drying and crushing, with its pulverizing, cross 200 mesh sieves, parallelly take by weighing 16 parts of beta-schardinger dextrin-cross-linked resins after sieving, every part of 0.1g joins respectively in the dry conical flasks of 16 250mL.Other prepares the goldstandard solution that gold ion concentration is respectively 25 μ g/L, 50 μ g/L, 75 μ g/L, 100 μ g/L, 150 μ g/L, 200 μ g/L, 250 μ g/L, 300 μ g/L, 350 μ g/L, 400 μ g/L, 450 μ g/L, 500 μ g/L, 600 μ g/L, 700 μ g/L, 800 μ g/L and 1000 μ g/L, be settled to 50mL with 2mol/L hydrochloric acid 2.5mL respectively again, pH value=1 of every part of goldstandard solution.Then 16 parts of goldstandard solution are joined respectively in the dry conical flask of above-mentioned 16 250mL, in the water bath with thermostatic control oscillator behind vibration 2h under rotating speed 200r/min, the 30 ℃ of conditions, take out respectively and by the filter bowl suction filtration of the method among the embodiment 1, make a series of enriched sample, with XRF the gained enriched sample is detected, adopts instrument condition parameter such as following table during detection:
| Element | U(KV) | I(mA) | Crystal | The θ angle | Line | BG | Time | detector | PHA |
| Au | 60 | 55 | 1∶LiF | 36.96 | Lα | 36.41-37.65 | 40 | SC | 26-78 |
Fig. 7 is that above-mentioned 16 enriched sample adopt XRF to detect the gained typical curve, and linear equation is y=0.006x-0.009, R
2=0.999, detect and be limited to 7.1 μ g/L.Good in the concentration range internal linear of broad as can be seen from Figure 7.Above result shows that the inventive method is applicable to the detection of XRF to trace gold in the sample, and detection limit is low.
Claims (9)
1. one kind is used for the preenrichment method for making sample that XRF detects trace noble metal, it is characterized in that may further comprise the steps at least:
(1) adding the capacity mass percent concentration in the container that fills beta-schardinger dextrin-is 30%～50% sodium hydroxide solution, vibrate in 40 ℃～60 ℃ waters bath with thermostatic control behind the mixing, after the transparent uniform solution to be formed, drip epichlorokydrin to reaction system, the amount ratio of beta-schardinger dextrin-and epichlorokydrin is 1g: 1～3mL, continue concussion, obtain the transparent gel-form product, the product taking-up is smashed to pieces,, behind acetone rinsing, dry again to neutral with distilled water flushing, obtain the beta-schardinger dextrin-cross-linked resin, put in the exsiccator preserve standby;
(2) dried beta-schardinger dextrin-cross-linked resin is pulverized, sieve, ratio in 1g: 0.5L～25L is mixed the beta-schardinger dextrin-cross-linked resin with the standard solution of precious metal element to be measured, the concentration of precious metal ion is 10 μ g/L～1000 μ g/L in the standard solution, fully after the vibration, with water system miillpore filter suction filtration, make enriched product attached to also evenly focusing in the survey area scope of XRF on the water system miillpore filter;
(3) will be attached with the water system miillpore filter tiling back oven dry of enriched product, obtain being used for the preenrichment sample that XRF detects trace noble metal.
2. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 1, it is characterized in that: the temperature of water bath with thermostatic control is 50 ℃ in the step (1).
3. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 1 is characterized in that: be that dried beta-schardinger dextrin-cross-linked resin is pulverized in the step (2), cross 160～200 mesh sieves.
4. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 1, it is characterized in that: fully vibrating in the step (2) is under the water bath with thermostatic control condition, and the temperature of water bath with thermostatic control is 15～40 ℃.
5. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 1, it is characterized in that: the suction filtration process is filter bowl to be placed carry out suction filtration on the core in the step (2), used filter bowl is made of and both ends open the upper cup and the bottom cup of hollow, the xsect at the arbitrary place of upper cup is circular, cross-sectional diameter from the top end opening of upper cup to the bottom end opening of upper cup reduces gradually, the bottom cup is cylindric, the bottom end opening equal diameters of the top end opening of bottom cup and upper cup, the top end opening of bottom cup are connected with the bottom end opening of upper cup makes upper cup and bottom cup form one.
6. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 5, it is characterized in that: the edge of the longitudinal section of upper cup is curved.
7. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 5, it is characterized in that: the longitudinal section of upper cup is inverted trapezoidal.
8. the preenrichment method for making sample that is used for XRF detection trace noble metal according to claim 5, it is characterized in that: the area of the xsect of bottom cup is no more than the survey area of XRF.
9. according to claim 5 or the 8 described preenrichment method for making sample that are used for XRF detection trace noble metal, it is characterized in that: the bottom end opening of bottom cup is a ground.
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| CN105319088A (en) * | 2014-06-25 | 2016-02-10 | 四川大学 | Pre-treatment method of detection of liquid sample with laser-induced breakdown spectroscopy |
| CN108844986A (en) * | 2018-06-28 | 2018-11-20 | 南京航空航天大学 | A kind of film method for making sample for trace plant sample EDXRF analysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102636505A (en) * | 2012-03-20 | 2012-08-15 | 中国科学院合肥物质科学研究院 | Method for synchronously detecting single-ion-beam and double-channel signals |
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| CN105319088A (en) * | 2014-06-25 | 2016-02-10 | 四川大学 | Pre-treatment method of detection of liquid sample with laser-induced breakdown spectroscopy |
| CN105319088B (en) * | 2014-06-25 | 2018-07-06 | 四川大学 | A kind of pre-treating method of laser induced breakdown spectroscopy detection fluid sample |
| CN104297276A (en) * | 2014-08-29 | 2015-01-21 | 无锡英普林纳米科技有限公司 | Method for analysis of trace elements in geological sample by X-fluorescence spectrum |
| CN108844986A (en) * | 2018-06-28 | 2018-11-20 | 南京航空航天大学 | A kind of film method for making sample for trace plant sample EDXRF analysis |
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Application publication date: 20111221 |