CN105388141A - Method for measuring gold element content in core-shell type gold-magnetic nano composite catalyst through inductively coupled plasma emission spectrum - Google Patents
Method for measuring gold element content in core-shell type gold-magnetic nano composite catalyst through inductively coupled plasma emission spectrum Download PDFInfo
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Abstract
The invention discloses a method for measuring gold element content in a core-shell type gold-magnetic nano composite catalyst through an inductively coupled plasma emission spectrum. Aqua regia, hydrofluoric acid and perchloric acid are added into a core-shell type gold-magnetic nano composite catalyst sample for heating and acidolysis, so that solid powder is completely dissolved, the transparent clear inorganic liquid is heated and evaporated to be nearly dry after being obtained, the volume of the sample solution is fixed through dilute nitric acid, and a sample blank is prepared through the same method; after work parameters of instruments are optimized, an inductively coupled plasma emission spectrograph is used for measuring the sample blank and a standard solution, and a gold element standard work curve is drawn; the inductively coupled plasma emission spectrograph is used for measuring light intensity of the core-shell type gold-magnetic nano composite catalyst sample solution, and the content of the gold element is obtained according to the drawn gold standard solution work curve and the light intensity of the sample solution. The method is easy, convenient, accurate and quick to operate, high in standard-adding recovery rate, good in repeatability and high in accuracy and precision.
Description
Technical field
The present invention relates to the method for gold element content in a kind of inductance Coupled Plasma-Emission spectroscopic assay core-shell type gold-magnetic Nano composite catalyst, belong to gold element detection technique field in core-shell type gold-magnetic Nano composite catalyst.
Background technology
By have excellent magnetic can magnetic nano-particle to combine with catalytic performance the magnetic Nano composite catalyst prepared, because it has, specific surface area is large, the undersaturated avtive spot of coordination of exposed surface is many, and the features such as simple separation are realized under additional magnetic fields, make magnetic Nano composite catalyst have the advantage such as high catalytic activity and easily separated recovery.Magnetic Nano composite granules coated with gold nano grain; magnetic nanoparticle can be protected from the interference of external environment; prevent its oxidation or reunite; a sp act surface can also be provided simultaneously; catalytic site is grafted on magnetic Nano composite granules; form core-shell type gold-magnetic Nano composite catalyst; it is as heterogeneous nucleophilic catalyst; there is good catalytic activity and returnability; and gold nano grain is as the active site of this type of catalyzer; to the mensuration of its content, directly affect the activity of catalyzer and the calculating of conversion ratio (TOF) thereof.Therefore, the content of gold element in Accurate Determining core-shell type gold-magnetic Nano composite catalyst, just seems particularly important.At present the mensuration of gold element content in core-shell type gold-magnetic Nano composite catalyst be have not been reported.
Inductive coupling plasma emission spectrograph (ICP-OES), because of advantages such as its detectability are low, precision is high, the mensuration linear dynamic range of concentration is wide, chemistry disruption is few, becomes the incomparable a kind of analysis means of other analytical technology in trace, measurement element determination.Method proposes by the acid-soluble processing sample of wet method, inductive coupling plasma emission spectrum method measures the method for gold element content in core-shell type gold-magnetic Nano composite catalyst.
Summary of the invention
The object of this invention is to provide a kind of easy, quick, accurate, adopt inductive coupling plasma emission spectrograph (ICP-OES) to measure the method for gold element content in core-shell type gold-magnetic Nano composite catalyst (concentration range is 6.0 ~ 300mg/g) reliably.
The preparation method of core-shell type gold-magnetic Nano composite catalyst: by sol-gal process at black Fe
3o
4nano grain surface parcel skim SiO
2, obtain Fe
3o
4siO
2nano particle, adds tetraethyl orthosilicate (TEOS) after being dissolved in ammoniacal liquor, stirring at room temperature 10 hours, then adds aminopropyl triethoxysilane (APTES) toluene solution, refluxes 10 hours, obtains Fe
3o
4siO
2-NH
2; By Fe
3o
4siO
2-NH
2with the gold nano grain (tetra chlorauric acid hydrogen (HAuCl of claret
44H
2o) aqueous solution and trisodium citrate (C
6h
5na
3o
72H
2o) be obtained by reacting) mixing, after ultrasonic disperse, stirring at room temperature 4 hours, obtains Fe
3o
4siO
2-Au magnetic nanometer composite material; By Fe
3o
4siO
2-Au is distributed in cetab (CTAB) ammonia spirit, adds TEOS, and stirring at room temperature 8 hours, obtains Fe
3o
4siO
2-AumSiO
2core-shell type gold-magnetic Nano composite catalyst.
A method for gold element content in inductance Coupled Plasma-Emission spectroscopic assay core-shell type gold-magnetic Nano composite catalyst, is characterized in that comprising the following steps:
1) 10.0 ~ 50.0mg(is accurate to 0.1mg) dry core-shell type gold-magnetic Nano composite catalyst solid powder sample is poured in polytetrafluoroethylene beaker, add 1 ~ 2mL one-level deionized water and soak sample, then 5 ~ 15mL chloroazotic acid of new preparation is added, 3 ~ 8mL hydrofluorite, 2 ~ 6mL perchloric acid, add and be placed on 120 ~ 180 DEG C of heat resolve until dissolution of solid is complete, after obtaining transparent clear inorganic liquid, uncap, slowly be warming up to 140 ~ 190 DEG C, emit the white cigarette of most perchloric acid, heating evaporation is to remaining 3mL, cooling, dilute nitric acid solution with 6% rinses wall of cup 4 ~ 5 times, reusable heat washing 3 ~ 4 times, solution is transferred in 25 or 50mL volumetric flask, be cooled to room temperature, scale is diluted to the dilute nitric acid solution of 3%, mix and obtain core-shell type gold-magnetic Nano composite catalyst sample solution, blank solution presses same method preparation,
2) preparation of standard solution: get respectively 50mg/L gold element standard solution 0,1.0,5.0,10.0mL is in 50mL volumetric flask, add 1 ~ 2mL red fuming nitric acid (RFNA), be diluted to scale with one-level deionized water, successively blank solution and concentration be 1.0,5.0, the standard series of 10.0mg/L, mixing;
3) drawing standard solution working curve: adopt Inductively coupled plasma optical emission spectrometer to measure above-mentioned blank solution, standard specimen solution respectively, draw out gold element standard solution working curve;
4) sample test: adopt Inductively coupled plasma optical emission spectrometer determination step 1) described in core-shell type gold-magnetic Nano composite catalyst sample solution, record by step 3) the content that gold element standard solution working curve calculates gold element in core-shell type gold-magnetic Nano composite catalyst.
The concentration of nitric acid of described step 1) preparation needed for chloroazotic acid is 68 ~ 70%, and concentration of hydrochloric acid is 36 ~ 38%; Hydrofluoric acid concentration is 48 ~ 50%, and perchloric acid concentration is 70%, and one-level deionized water resistivity is 18.25M Ω cm(25 DEG C).
In described step 4), in core-shell type gold-magnetic Nano composite catalyst, the concentration range of gold element is 6.0 ~ 300mg/g.
The running parameter of described Inductively coupled plasma optical emission spectrometer is: the analytical line of gold element: 211.068nm, 242.794nm, 267.594nm; Emissive power: 1.25kW; Height of observation: 12mm; Atomization gas flow: 0.50L/min; Plasma gas flow rate: 15.0L/min; Assisted gas flow: 1.50L/min; Peristaltic pump speed: 15rpm; Sample introduction time delay: 30s.
In nano catalyst, gold element content is calculated as follows:
C=(Ci－C0)×V/M；
In formula: the content (mg/g) of gold element in C---catalyzer; The content of this element of Ci---in test solution (mg/L); The content of this element of C0---in blank solution (mg/L); The volume (L) of V---test solution; M---takes the quality (g) of catalyst sample.
The technical identification of this method: carried out the detection limits of this method, mark-on recovery, repeatability, internal standard method, serial dilution experiment respectively with Inductively coupled plasma optical emission spectrometer, demonstrated this method and there is higher accuracy and precision.
Embodiment
1 experiment material
1.1 key instruments and equipment
Inductive coupling plasma emission spectrograph (ICP-OES): Agilent company of the U.S., 725-ES type, CCD detecting device covers from the whole wavelength coverage of 167-785nm;
Laboratory Superpure water machine: Molecular company, atom type 1810D, one-level deionized water resistivity (25 DEG C) is 18.25M Ω cm;
Electronic balance: MettlerToledo company, XP6 type, range of weighing is 0.001mg ~ 6.0g;
Anticorrosion electric hot plate: strand plastic instrument factory at prime, DBF-1 type, temperature range is 0-200 DEG C.
1.2 main agents
Nitric acid: ACS level reagent, 68-70%, density is 1.41g/mL, ACROS company;
Hydrochloric acid: analytical reagent, 36-38%, density is 1.26g/mL, Xi Long chemical company;
Hydrofluorite: ACS level reagent, 48-50%, density is 1.15g/mL, lark prestige company;
Perchloric acid: ACS level reagent, 70%, density is 1.66g/mL, lark prestige company;
One-level deionized water: by the self-control of Molecular laboratory Superpure water machine, resistivity (25 DEG C) is 18.25M Ω cm;
Standard reserving solution: gold element standard solution 1000mg/L, national non-ferrous metal and electronic material Institute of Analysis; Goldstandard storing solution is diluted to 50mg/L for subsequent use, during mensuration stepwise dilution become 0.5,1.0,2.0,5.0, the standard series of 10.0mg/L.
The Instrument working parameter of 1.3ICP-OES
The analytical line of gold element: 211.068nm, 242.794nm, 267.594nm;
Emissive power: 0.9 ~ 1.5kW;
Height of observation: 5 ~ 15mm;
Atomization gas flow: 0.4 ~ 1.4L/min;
Plasma gas flow rate: 10.0 ~ 20.0L/min;
Assisted gas flow: 0.75 ~ 2.25L/min;
Peristaltic pump speed: 15rpm;
Sample introduction time delay: 30s;
2 experimental procedures
2.1 sample pre-treatments
Core-shell type gold-magnetic Nano composite catalyst solid powder sample the 31.0mg(accurately taking oven dry is accurate to 0.1mg) in 50mL polytetrafluoroethylene beaker, add 1 ~ 2mL one-level deionized water and soak sample, slowly add new preparation 8mL chloroazotic acid, 4mL hydrofluorite, 3mL perchloric acid, add a cover and be placed on electric heating temperature control plate, in 150 DEG C of heat resolve 1.5h, until dissolution of solid is complete, after obtaining transparent clear inorganic liquid, uncap, slowly be warming up to 170 DEG C, emit the white cigarette of most perchloric acid, heating evaporation is near dry, take off polytetrafluoroethylene beaker, cooling, wall of cup is rinsed 4 ~ 5 times with 6% dilute nitric acid solution, reusable heat washing 3 ~ 4 times, solution is moved in 25mL volumetric flask, be cooled to room temperature, scale is diluted to 3% dilute nitric acid solution, mixing, to be measured.Sample blank presses same method preparation.
The preparation of 2.2 standard solution
Gold element standard reserving solution is national standard reagent, and concentration is 1000mg/L, gold element standard reserving solution is diluted to 50mg/L with 2% nitric acid for subsequent use.During mensuration stepwise dilution become 0.5,1.0,2.0,5.0, the standard series of 10.0mg/L.
2.3 instrument conditions of work are optimized
2.3.1 the selection of instrument power
Employing concentration is the goldstandard solution of 5.0mg/L, carries out power selection at 0.9 ~ 1.5kW.The signal background ratio measured shows, improves power, and signal value increases, but background value also increases.Final optimization pass is the power of 1.25kW.
2.3.2 the selection of atomization gas flow
Employing concentration is the goldstandard solution of 5.0mg/L, carries out the selection of atomization gas flow at 0.4 ~ 1.4L/min.Signal to background ratio shows, increases atomization gas flow, and signal value increases, but Matrix effects also corresponding increase.Final optimization pass is the atomization gas flow of 0.5L/min.
2.3.3 the selection of observed altitude
Employing concentration is the goldstandard solution of 5.0mg/L, carries out observed altitude selection at 5 ~ 15mm.Final optimization pass is the observed altitude of 12mm.
2.3.4 Instrument working parameter
Sensitivity selection determination and analysis line according to gold element spectral line is: 211.068nm, 242.794nm and 267.594nm.
Table 1 instrument Optimization Work parameter
The foundation of 2.4 typical curves
According to above-mentioned instrument condition of work, the standard solution of gold element 4 concentration point is measured, draw the standard solution working curve of gold element.Simultaneously to sample blank solution METHOD FOR CONTINUOUS DETERMINATION 10 times, by formula
dL=
kScalculate its detection limit (in formula, S is the standard deviation of 10 blank solution test concentrations).Analysis result shows: each elemental standards curve linear related coefficient is all between 0.991 ~ 0.999, and assay method linear relationship is good.
2.5 sample tests
Inductive coupling plasma emission spectrograph is under above-mentioned running parameter, and adopt calibration curve method, carry out assay to the gold element in gold-magnetic Nano composite catalyst sample, every increment product replicate determination 3 times, averages; Obtain the levels of Gold Samples element according to the working curve of goldstandard solution and the light intensity of solution to be measured, the data after mensuration, through formula scales, can obtain the content of gold element in gold-magnetic Nano composite catalyst.
In gold-magnetic Nano composite catalyst, gold element content is calculated as follows:
C=(Ci－C0)×V/M
In formula: the content (mg/g) of gold element in C---catalyzer;
The content of this element of Ci---in test solution (mg/L);
The content of this element of C0---in blank solution (mg/L);
The volume (L) of V---test solution;
M---takes the quality (g) of catalyst sample;
Calculate the content (mg/g) of gold element in raw catalyst.
Embodiment 1
Core-shell type gold-magnetic Nano composite catalyst solid powder sample the 45.0mg(accurately taking oven dry is accurate to 0.1mg) in 50mL polytetrafluoroethylene beaker, add 1 ~ 2mL one-level deionized water and soak sample, slowly add new preparation 8mL chloroazotic acid, 4mL hydrofluorite, 3mL perchloric acid, add a cover and be placed on electric heating temperature control plate, in 150 DEG C of heat resolve 1.5h, until dissolution of solid is complete, after obtaining transparent clear inorganic liquid, uncap, slowly be warming up to 170 DEG C, emit the white cigarette of most perchloric acid, heating evaporation is to remaining 3mL, take off polytetrafluoroethylene beaker, cooling, wall of cup is rinsed 4 ~ 5 times with 6% dilute nitric acid solution, reusable heat washing 3 ~ 4 times, solution is moved in 50mL volumetric flask, be cooled to room temperature, scale is diluted to 3% dilute nitric acid solution, mixing, to be measured.Inductive coupling plasma emission spectrograph is utilized to measure the light intensity of sample solution, the levels of gold element is obtained according to the standard solution working curve of gold element and the light intensity of gold to be measured-magnetic Nano composite catalyst sample solution, through calculating, the average content obtaining gold element in testing sample is 34.66mg/g(3.466%).
Embodiment 2
Accurately take core-shell type gold-magnetic Nano composite catalyst pressed powder that 31.0mg is dried, utilize the sampler-dissolving method described in embodiment 1 to produce gold to be measured-magnetic Nano composite catalyst sample solution, constant volume is in 25mL volumetric flask.Inductive coupling plasma emission spectrograph is utilized to measure the light intensity of sample solution, the levels of gold element is obtained according to the standard solution working curve of gold element and the light intensity of gold to be measured-magnetic Nano composite catalyst sample solution, through calculating, the average content obtaining gold element in testing sample is 34.03mg/g(3.403%).
3 embodiment technical identifications:
3.1 detection limit experiments
By the concentration of 10 replicate determination blank solutions, by formula
dL=
kScalculate its detection limit (in formula, S is the standard deviation of 10 blank solution test concentrations), get 3 times of standard deviations of testing result as detection limits, 10 times of standard deviations are as quantitative limit (LOQ Limitsofquantification).
The mensuration (n=10, mg/L) of table 2 detection limit
From table 2, this method measures detecting of gold element and is limited to 0.041mg/L.
The mensuration of 3.2 accuracy
3.2.1 recovery testu
For investigating the reliability of this method, using the instrument condition of work described in step 3, measuring the content of gold element in gold-magnetic Nano composite catalyst sample solution, add the standard solution of gold element more in the sample to which, measure its alluvial, calculate recovery of standard addition, the results are shown in Table 3.
Table 3 recovery is tested
Recovery of standard addition=(mark-on Specimen Determination value-Specimen Determination value) ÷ adds scalar × 100%;
From the result of table 3, the recovery of gold element, between 98 ~ 102%, meets test request.
3.2.2 serial dilution experiment
Table 4 serial dilution is tested
Measured value after theoretical value ÷ dilution after linearly dependent coefficient=dilution;
From the result of table 4, good linear relationship should be kept between the signal intensity of gold element and matrix concentration, meet test request.
3.2.3 internal standard method is tested:
In order to the error that the matrix effect of rectify an instrument moment or long-term drift and sample is brought, adopt metallic yttrium (Y) to carry out internal standard method experiment for interior mark, the results are shown in Table 5, the analytical line of yttrium does not have overlapping with the spectral line of gold element, noiseless;
Table 5 internal standard method is tested
From the result of table 5, the sample matrices interference in this method does not almost have, negligible.
3.3 repeated experiment
By core-shell type gold-magnetic Nano composite catalyst sample solution replicate determination 10 times, calculate the precision that relative standard deviation determines gold element in the method, the results are shown in Table 6.
The precision of table 6 method
From the result of table 6, the relative standard deviation of this method is 1.540%, shows that the precision of this method is better.
Claims (4)
1., by a method for gold element content in inductance Coupled Plasma-Emission spectroscopic assay core-shell type gold-magnetic Nano composite catalyst, it is characterized in that comprising the following steps:
1) by 10.0 ~ 50.0mg dry core-shell type gold-magnetic Nano composite catalyst solid powder sample is poured in polytetrafluoroethylene beaker, add 1 ~ 2mL one-level deionized water and soak sample, then 5 ~ 15mL chloroazotic acid of new preparation is added, 3 ~ 8mL hydrofluorite, 2 ~ 6mL perchloric acid, add and be placed on 120 ~ 180 DEG C of heat resolve until dissolution of solid is complete, after obtaining transparent clear inorganic liquid, uncap, slowly be warming up to 140 ~ 190 DEG C, emit the white cigarette of most perchloric acid, heating evaporation is to remaining 3mL, cooling, dilute nitric acid solution with 6% rinses wall of cup 4 ~ 5 times, reusable heat washing 3 ~ 4 times, solution is transferred in 25 or 50mL volumetric flask, be cooled to room temperature, scale is diluted to the dilute nitric acid solution of 3%, mix and obtain core-shell type gold-magnetic Nano composite catalyst sample solution, blank solution presses same method preparation,
2) preparation of standard solution: get respectively 50mg/L gold element standard solution 0,1.0,5.0,10.0mL is in 50mL volumetric flask, add 1 ~ 2mL red fuming nitric acid (RFNA), be diluted to scale with one-level deionized water, successively blank solution and concentration be 1.0,5.0, the standard series of 10.0mg/L, mixing;
3) drawing standard solution working curve: adopt Inductively coupled plasma optical emission spectrometer to measure above-mentioned blank solution, standard specimen solution respectively, draw out gold element standard solution working curve;
4) sample test: adopt Inductively coupled plasma optical emission spectrometer determination step 1) described in core-shell type gold-magnetic Nano composite catalyst sample solution, record by step 3) the content that gold element standard solution working curve calculates gold element in core-shell type gold-magnetic Nano composite catalyst.
2. the method for claim 1, it is characterized in that the concentration of nitric acid of described step 1) preparation needed for chloroazotic acid is 68 ~ 70%, concentration of hydrochloric acid is 36 ~ 38%; Hydrofluoric acid concentration is 48 ~ 50%, and perchloric acid concentration is 70%, and the resistivity of one-level deionized water 25 DEG C time is 18.25M Ω cm.
3. the method for claim 1, is characterized in that the concentration range of gold element in core-shell type gold-magnetic Nano composite catalyst in described step 4) is 6.0 ~ 300mg/g.
4. the method for claim 1, is characterized in that the running parameter of described Inductively coupled plasma optical emission spectrometer is: the analytical line of gold element: 211.068nm, 242.794nm, 267.594nm; Emissive power: 1.25kW; Height of observation: 12mm; Atomization gas flow: 0.50L/min; Plasma gas flow rate: 15.0L/min; Assisted gas flow: 1.50L/min; Peristaltic pump speed: 15rpm; Sample introduction time delay: 30s.
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