CN112147118A - Method for determining 34 elements in geochemical sample - Google Patents
Method for determining 34 elements in geochemical sample Download PDFInfo
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- CN112147118A CN112147118A CN202010996793.2A CN202010996793A CN112147118A CN 112147118 A CN112147118 A CN 112147118A CN 202010996793 A CN202010996793 A CN 202010996793A CN 112147118 A CN112147118 A CN 112147118A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention relates to a method for measuring 34 elements in a geochemical sample, which adopts inverted aqua regia, hydrofluoric acid and perchloric acid to treat the sample, and the inverted aqua regia is extracted. According to the method for measuring 34 elements in the geochemical sample, the sample is pretreated by the reverse aqua regia, the tetraacid is used for dissolving the ore, the reverse aqua regia is used for extracting, the 34 elements can be measured simultaneously, the ore melting method replaces various ore melting methods in a multi-target matching scheme, the working efficiency is improved, and the experiment cost is saved.
Description
Technical Field
The invention relates to the technical field of environmental engineering, in particular to a method for determining 34 elements in a geochemical sample.
Background
According to a multi-target matching scheme, the Se determination method comprises the steps of decomposing nitric acid-perchloric acid and determining by using an atomic fluorescence spectrometry in a hydrochloric acid medium; s adopts a combustion-iodometry method; al, Rb, Mo, Li, Be, Ca, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Na, Mg, P, K, Fe, U, Tl, La, Ce are measured by powder tablet-X-ray fluorescence spectrometry or nitric acid-hydrochloric acid-perchloric acid-hydrofluoric acid tetraacid decomposition-inductively coupled plasma emission spectrometry or nitric acid-hydrofluoric acid-perchloric acid triacid decomposition-inductively coupled plasma mass spectrometry.
At present, various pretreatment ore melting methods are needed to complete analysis tasks when the elements are related, and the investment of manpower and material resources is large.
Disclosure of Invention
The embodiment of the invention provides a method for measuring 34 elements in a geochemical sample, which can be used for measuring 34 elements simultaneously, improves the working efficiency and saves the experiment cost.
The embodiment of the invention provides a method for measuring 34 elements in a geochemical sample, which comprises the steps of treating the sample by using reverse aqua regia, hydrofluoric acid and perchloric acid, and extracting the reverse aqua regia. The inventor finds that after the sample is pretreated by the reverse aqua regia, the tetraacid is used for dissolving the ore, the reverse aqua regia is used for extracting, 34 elements (Se, S, Al, Rb, Mo, Li, Be, Ca, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Na, Mg, P, K, Fe, Tl, U, La and Ce) can Be simultaneously measured, and a ore melting method is used for replacing various ore melting methods in a multi-target matching scheme, so that the working efficiency is improved, and the experimental cost is saved.
In some preferred embodiments, the sample is pretreated by adding the reverse aqua regia, and then the mixed acid of the hydrofluoric acid and the perchloric acid is added for reaction, and then the reverse aqua regia is used for extraction.
In some preferred embodiments, the mass-to-volume ratio of the sample to the reverse aqua regia in the pretreatment is 0.2-0.3 g: 5-20 mL. Preferably, the mass-to-volume ratio of the sample to the reverse aqua regia is 0.25g to 10 mL.
In some preferred embodiments, the mass-to-volume ratio of the sample to the mixed acid is 0.2-0.3 g: 5-20 mL. Preferably, the mass-to-volume ratio of the sample to the mixed acid is 0.25g:10 mL.
In some preferred embodiments, the volume ratio of the hydrofluoric acid to the perchloric acid in the mixed acid is 4-7: 1-4. Preferably, the volume ratio of the hydrofluoric acid to the perchloric acid is 5: 2.
In some preferred embodiments, 0.2-0.3 g of the sample is weighed, water is added for wetting, 5-20 mL of reverse aqua regia is added, the temperature is raised to 120-150 ℃, and the temperature is controlled for dissolving for 30-90 min; and adding 5-20 mL of mixed acid, continuously heating to preferably 250-300 ℃, evaporating until white smoke is emitted, controlling the temperature to be 120-160 ℃, preferably until the temperature is evaporated to dryness, extracting with 5-15 mL of reverse aqua regia, and keeping the temperature for 5-10 min. Preferably, 0.2500g of sample is weighed and put into a polytetrafluoroethylene crucible, a small amount of water such as 1-3 mL of wetting is added, 10mL of reverse aqua regia is added, the mixture is placed on an electric hot plate for low-temperature heating, and the temperature is controlled for dissolution for 1 hour. Then 10mL of mixed acid (VHF: VHClO) was added4And (5: 2), continuously heating and evaporating until white smoke is emitted, controlling the temperature to be about 130-150 ℃ until the white smoke is evaporated to dryness, extracting with 10mL1:1 reverse aqua regia, preserving the heat for 10min, taking down, cooling, transferring into a 25mL colorimetric tube, diluting with deionized water to a scale, and shaking uniformly to be detected.
In some preferred embodiments, Se is determined using atomic fluorescence spectroscopy; inductively coupled plasma spectroscopy and inductively coupled plasma mass spectrometry were used to determine 33 elements other than Se: s, Al, Rb, Mo, Li, Be, Ca, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Na, Mg, P, K, Fe, Tl, U, La and Ce; preferably, one or more of S, Al, Ca, Fe, Mg, Na, P and K is measured by inductively coupled plasma spectrometry; and/or measuring one or more of Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Tl, La, Rb, U, Ce and Mo by adopting an inductively coupled plasma mass spectrometry method.
In some preferred embodiments, the operating parameters of the inductively coupled plasma mass spectrometer used include: the power is 1550w, the sampling pump speed is 40r/min, the cooling gas flow is 14L/min, the sampling flushing time is 20s, the auxiliary gas flow is 0.8L/min, the scanning mode is peak jump, the atomizer flow is 1.14L/min, and the scanning times are 50 times.
In some preferred embodiments, the operating parameters of the inductively coupled plasma spectroscopy employed include: the negative high pressure is 270V, the atomization method is a flame method, the lamp current is 80mA, the reading mode is a peak area, the furnace temperature is 300 ℃, the sampling time is 10s, the height of the atomizer is 5mm, the reading time is 16s, the carrier gas flow is 800mL/min, the delay time is 3s, the auxiliary gas flow is 300mL/min, and the pump speed is 100 r/min.
In some preferred embodiments, the operating parameters of atomic fluorescence employed include: power 1150w, sample pump speed 40r/min, vertical observation height 12mm, atomizer pressure 0.3MPa, auxiliary gas flow 0.8L/min, integration time 2 s.
According to the invention, 34 elements can be simultaneously measured by adopting the method, one ore melting method replaces various pretreatment ore melting methods in a multi-target matching scheme, and on the premise of meeting the detection limit, precision and accuracy of experimental requirements, the complex operation and the large amount of the consumption of nitric acid, hydrochloric acid, hydrofluoric acid and perchloric acid are reduced, the efficiency is increased, the experimental cost is saved, and the environmental pollution is reduced.
The invention has the beneficial effects that: after the sample is pretreated by the reverse aqua regia, the tetraacid is dissolved in the ore, the temperature is controlled and the water is evaporated to dryness, the reverse aqua regia is extracted, 34 elements can be simultaneously measured, and the ore melting method replaces various ore melting methods in a multi-target matching scheme, so that the working efficiency is improved, and the experimental cost is saved. The accuracy, precision and detection limit of the method at least meet the standard of DZ/T0130.5-2006 geological mineral laboratory test quality standard.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
In the present invention, the instruments and the like used are conventional products which are purchased from regular vendors, not indicated by manufacturers. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature.
In the following examples, the main reagents such as hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid, potassium borohydride, potassium hydroxide are analytically pure, and the experimental water is distilled water; fe3+Salt solution (25 mg/mL): 121g of ferric chloride (FeCl)3·6H2O) is dissolved in 200mL (1+1) HCI, transferred into a 1000mL volumetric flask, supplemented with 300mL hydrochloric acid, subjected to constant volume and shaken up.
In the following examples, the detection instrument used was: iCAPQa inductively coupled plasma mass spectrometer (thermoelectric corporation, usa). AF-640A atomic fluorescence spectrometer (Beijing Rayleigh Analyzer Co.); selenium high-strength hollow cathode lamp carrying 10% hydrochloric acid. iCAP-6300 inductively coupled plasma Spectroscopy (thermoelectric corporation, USA).
In the following examples, during inductively coupled plasma mass spectrometry, a solution to be measured is introduced into a radio frequency plasma in a pneumatic atomization mode, separation detection is performed by using a quadrupole inductively coupled plasma mass spectrometer according to different example mass-to-nuclear ratios of elements after evaporation, atomization and ionization, and rhodium is used as an internal standard for correction to obtain the content of each element. During atomic fluorescence measurement, selenium and potassium borohydride react in a hydrochloric acid solution to generate hydride gas, argon is used as carrier gas, a selenium high-intensity hollow cathode lamp is used for exciting a light source, a characteristic spectral line of selenium is emitted, the fluorescence intensity of the selenium is measured on an atomic fluorescence spectrometer and is compared with the fluorescence intensity of a calibration working solution, and the content of the selenium in a sample is calculated. And during the inductively coupled plasma spectrometry, measuring the characteristic spectral intensity of the component to be measured in the sample solution by using an inductively coupled plasma emission spectrometer at a specified wavelength, and calculating the content of the component to be measured in the sample.
In the following examples, the operating parameters for the specific tests employed are as follows: the operating conditions of the inductively coupled plasma mass spectrometer are shown in table 1. The operating parameters of the atomic fluorescence spectrometer are shown in table 2 (10% hydrochloric acid carried). The operating conditions of the inductively coupled plasma spectrometer are shown in table 3. Standard solution: the rhodium internal standard mother liquor is 1000 mug/mL and is diluted by water to the working solution concentration of 10 ng/mL. The standard solution is purchased by the national iron and steel testing center. For convenience of use, the element standard solution is prepared into standard use solution.
TABLE 1 inductively coupled plasma Mass spectrometer operating parameters
| Operating parameters | Set value | Operating parameters | Set value |
| Power of | 1550w | Speed of sample pump | 40r/min |
| Flow of cooling gas | 14L/min | Sample injection and flushing time | 20s |
| Auxiliary gas flow | 0.8L/min | Scanning mode | Jumping peak |
| Flow rate of atomizer | 1.14L/min | Number of scans | 50 |
TABLE 2 atomic fluorescence working parameters
| Operating parameters | Condition | Operating parameters | Condition |
| Negative high pressure | 270V | Atomization method | Flame method |
| Lamp current | 80mA | Reading mode | Peak area |
| Furnace temperature | 300℃ | Sampling time | 10s |
| Atomizer altitude | 5mm | Time of reading | 16s |
| Flow of carrier gas | 800mL/min | Delay time | 3s |
| Auxiliary gas flow | 300mL/min | Speed of pump | 100r/min |
TABLE 3 inductively coupled plasma Spectrum operating parameters
| Operating parameters | Set value | Operating parameters | Set value |
| Power of | 1150w | Speed of sample pump | 40r/min |
| Vertical observation height | 12mm | Atomizer pressure | 0.3MPa |
| Auxiliary gas flow | 0.8L/min | Integration time | 2s |
Example 1
This example provides a method for determining 34 elements in a geochemical sample. The method comprises the following specific steps:
weighing 0.2500g of sample in a polytetrafluoroethylene crucible, adding a small amount of water or 1-3 mL of water for wetting, adding 10mL of reverse aqua regia, placing on an electric hot plate, heating at 130 ℃, and controlling the temperature to dissolve for 1 h. 10mL of mixed acid (V) was addedHF:VHClO4And (5: 2), continuously heating to 280 ℃, evaporating until white smoke is emitted, controlling the temperature at 140 ℃ until the smoke is evaporated to dryness, extracting with 10mL of reverse aqua regia (the volume ratio of nitric acid, hydrochloric acid and water is 3+1+4), preserving the heat for 10min, taking down, cooling, transferring into a 25mL colorimetric tube, diluting to a scale with deionized water, and shaking uniformly to be detected.
Adding 0.5ml Fe into 10ml of subareas3+Salt solution, and measuring Se in the solution by using atomic fluorescence spectrometry.
And measuring S, Al, Ca, Fe, Mg, Na, P and K in the stock solution by using inductively coupled plasma spectroscopy.
5mL of solution to Be detected is divided and diluted to 10mL, and Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Tl, La, Rb, U, Ce and Mo in the stock solution are measured by inductively coupled plasma mass spectrometry.
According to the experimental method of example 1, the national standard substances GSD-9, GSS-16 and GSD-17 were selected and measured for 12 times to determine the accuracy and precision of the method, and 12 blank solutions were prepared at the same time, and the detection limit was calculated by three times the standard deviation (3S), and the accuracy, precision and detection limit measurement results of the measurement method in this example are shown in Table 4.
TABLE 4 accuracy, precision and detection limits of the determination methods in example 1
Note: "+" indicates percent.
As can be seen from Table 4, the accuracy, precision and detection limit of the method for determining each element at least meet the standard of DZ/T0130.5-2006 geological mineral laboratory test quality Standard. Wherein the accuracy requirement is: within three times of detection limit, the delta lgC is less than or equal to 0.1, more than three times of detection limit, the delta lgC is less than or equal to 0.05, and the delta lgC is more than 1 percent and less than or equal to 0.04. The RSD percent within the precision three times detection limit is less than or equal to 14, the RSD percent above the three times detection limit is less than or equal to 10, and the RSD percent more than 1 percent is less than or equal to 8.
Comparative example 1
This comparative example experiment provides a method for determining 34 elements in a geochemical sample, which differs from example 1 in that: no adverse aqua regia was added.
Comparative example 2
This comparative example experiment provides a method for determining 34 elements in a geochemical sample, which differs from example 1 in that: the mixed solution of hydrofluoric acid and perchloric acid is replaced by the mixed solution of nitric acid and perchloric acid.
Comparative example 3
This comparative example experiment provides a method for determining 34 elements in a geochemical sample, which differs from example 1 in that: finally, the evaporating temperature is controlled at 250 ℃.
Compared with the comparative example, the method has the advantages that the reverse aqua regia is adopted for pre-digestion, the four-acid open ore melting, the low-temperature acid dispelling and the reverse aqua regia extraction in the example 1, and one ore melting method replaces multiple ore melting methods in a multi-target matching scheme, so that the working efficiency is improved, and the experiment cost is saved. And example 1 is superior in terms of accuracy, precision, detection limit.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for determining 34 elements in a geochemical sample is characterized in that the sample is treated by adopting reverse aqua regia, hydrofluoric acid and perchloric acid, and the reverse aqua regia is extracted.
2. The method according to claim 1, wherein said sample is pretreated by adding aqua regia, then said mixed acid of hydrofluoric acid and perchloric acid is added for reaction, and then said sample is extracted by adding aqua regia.
3. The method according to claim 2, wherein the mass-to-volume ratio of the sample to the retrograde aqua regia in the pretreatment is 0.2 to 0.3g:5 to 20 mL.
4. The method for determining 34 elements in a geochemical sample according to claim 1, wherein the mass to volume ratio of the sample to the mixed acid is 0.2-0.3 g: 5-20 mL.
5. The method for detecting 34 elements in a geochemical sample according to claim 2, wherein the volume ratio of the hydrofluoric acid to the perchloric acid in the mixed acid is 4-7: 1-4.
6. The method for determining 34 elements in a geochemical sample according to any one of claims 1-5, wherein 0.2-0.3 g of the sample is weighed, 1-3 mL of water is added for wetting, 5-20 mL of reverse aqua regia is added, the temperature is raised to 120-150 ℃, and the temperature is controlled for dissolving for 30-90 min; and adding 5-20 mL of mixed acid, continuously heating to 250-300 ℃, controlling the temperature to be 120-160 ℃, extracting with 5-15 mL of reverse aqua regia, and keeping the temperature for 5-10 min.
7. The method for determining 34 elements in a geochemical sample according to any one of claims 1-5, wherein Se is determined by atomic fluorescence spectroscopy; inductively coupled plasma spectroscopy and inductively coupled plasma mass spectrometry were used to determine 33 elements other than Se: s, Al, Rb, Mo, Li, Be, Ca, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Sr, Cd, Sb, Cs, Ba, W, Pb, Bi, Na, Mg, P, K, Fe, Tl, U, La and Ce.
8. The method of claim 7, wherein the operating parameters of inductively coupled plasma mass spectrometry used comprise: the power is 1550w, the sampling pump speed is 40r/min, the cooling gas flow is 14L/min, the sampling flushing time is 20s, the auxiliary gas flow is 0.8L/min, the scanning mode is peak jump, the atomizer flow is 1.14L/min, and the scanning times are 50 times.
9. The method of claim 7, wherein the operating parameters of the inductively coupled plasma spectroscopy used comprise: the negative high pressure is 270V, the atomization method is a flame method, the lamp current is 80mA, the reading mode is a peak area, the furnace temperature is 300 ℃, the sampling time is 10s, the height of the atomizer is 5mm, the reading time is 16s, the carrier gas flow is 800mL/min, the delay time is 3s, the auxiliary gas flow is 300mL/min, and the pump speed is 100 r/min.
10. The method of claim 7, wherein the operating parameters of atomic fluorescence employed comprise: power 1150w, sample pump speed 40r/min, vertical observation height 12mm, atomizer pressure 0.3MPa, auxiliary gas flow 0.8L/min, integration time 2 s.
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Citations (2)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110672707A (en) * | 2019-09-25 | 2020-01-10 | 中化地质矿山总局地质研究院 | Method for measuring boron, arsenic, bromine and tungsten in geochemical sample by ICP-MS |
| CN110715913A (en) * | 2019-10-10 | 2020-01-21 | 中化地质矿山总局地质研究院 | Method for measuring selenium in geochemical sample by atomic fluorescence spectrometry |
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