CN116067918A - Atomic emission spectrum carrier distillation buffer and preparation method thereof - Google Patents
Atomic emission spectrum carrier distillation buffer and preparation method thereof Download PDFInfo
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- CN116067918A CN116067918A CN202211541597.1A CN202211541597A CN116067918A CN 116067918 A CN116067918 A CN 116067918A CN 202211541597 A CN202211541597 A CN 202211541597A CN 116067918 A CN116067918 A CN 116067918A
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Abstract
The invention relates to a preparation method of an atomic emission spectrum carrier distillation buffer, firstly, crude silicon dioxide and carbon powder are respectively mixed with potassium pyrosulfate and ground uniformly; weighing sulfur powder, calcium carbonate, ferric oxide and polytetrafluoroethylene, mixing in a mortar, and fully grinding; then, respectively weighing analytically pure barium carbonate and spectrally pure barium carbonate, adding 0.7000g of silicon dioxide containing 1% of germanium dioxide internal standard substance, and mixing in a mortar; and finally, mixing the mixture obtained in the steps with white fine silica, sodium fluoride and alumina, putting the mixture into a mortar, fully grinding and uniformly mixing, and shaking and drying the mixture to obtain the spectrum carrier buffer. The atomic emission spectrum carrier buffer prepared by the method can rapidly promote oxidation, fluorination and vulcanization reactions of elements such as silver, boron, molybdenum, tin, lead and the like in a sample, and simultaneously the single-electrode carrier distillation method can improve the sensitivity of the element to be detected and the accuracy of an analysis result.
Description
Technical Field
The invention relates to a preparation method of an atomic emission spectrum carrier distillation buffer, belonging to the technical field of preparation of spectrum buffers.
Background
Since buffers are critical factors to ensure the stability of the emission spectrum light source. Under the condition of the determination of the instrument, the blank value directly determines the detection limit of the regional mine adjustment sample. The current working areas of the natural resource comprehensive investigation command center comprise Tibet, xinjiang, daxingan, sanjiang upstream areas, wuMongshan mining area and the like, and the background values of silver, molybdenum, boron, tin and lead in most working areas are relatively low. Only one gallery chemical research institute supplies the buffer, the blank value of boron exceeds 5ug/g in recent years, and the stability of a light source is poor, so that the qualification rate of primary results of silver and boron in mining samples of a plurality of laboratory areas in China is lower than 90%, and the reporting rate of the results of boron in partial working areas is lower than 85%, thereby directly affecting the imaging quality of regional geological mineral investigation work.
The special emission spectrometer of AES-7200 geological samples newly developed by Beijing Rayleigh analysis instrument company simplifies the complicated operation procedure of the traditional grating spectrograph, realizes the rapid determination of elements such as silver, boron, molybdenum, tin, lead and the like in powdery silicate geochemical samples, is limited by a recommended carrier buffer in literature, and has unsatisfactory effect on analysis of carbonate and high-speed railway silicate geochemical samples.
Disclosure of Invention
In order to solve the problems and the shortcomings of the prior art, the invention provides an atomic emission spectrum carrier buffer and a preparation method thereof. The spectrum carrier buffer prepared by the method can promote the oxidation, fluorination, and vulcanization reactions of elements such as silver, boron, molybdenum, tin, lead and the like in a sample within 30S, and the sensitivity of the element to be detected and the accuracy of an analysis result can be improved by using an AES-7200 geological sample special-purpose emission spectrometer by using a single-electrode carrier distillation method.
An atomic emission spectrum carrier buffer, its preparation method, the concrete step is as follows:
(1) Firstly, accurately weighing potassium pyrosulfate (K) by an electronic balance 2 S 2 O 7 ) 4.0g to 20.0g of the mixture is placed in an agate mortar and ground into white fine powder.
(2) The crude Silica (SiO) was re-weighed in order 2 ) 0.6 to 3.0g and 1.0 to 5.0g of carbon powder (C) are respectively mixed with potassium pyrosulfate and ground uniformly.
(4) Analytically pure barium carbonate (BaCO) was weighed separately 3 ) 1.0 to 5.0g and spectrally pure barium carbonate (BaCO) 3 ) 1.0 to 5.0g of silicon dioxide (SiO) containing 1 percent of germanium dioxide internal standard substance 2 ) 0.7g of the mixture is uniformly mixed in a mortar; white fine-grained Silica (SiO) 2 ) 1.4 to 7.0g and 0.86 to 4.3g of sodium fluoride (NaF) are added into the mixture for full grinding.
(5) Placing the above three ground mixtures in a clean agate tank, and weighing aluminum oxide (Al 2 O 3 ) 8.0g to 40.0g of powder are added into an agate tank together, and a proper amount of agate beads are put into the agate tank to be uniformly mixed on a ball mill.
(6) And (3) drying the final mixture obtained in the step (5) at 40-60 ℃ for 12 hours to obtain the spectrum carrier buffer.
And (3) in the steps (1), (2), (3), (4) and (5), the specifications of potassium pyrosulfate, carbon powder, sulfur powder, calcium carbonate, ferric oxide, polytetrafluoroethylene, sodium fluoride, aluminum oxide and germanium dioxide are analytically pure.
The silicon dioxide in the steps (2) and (4) is two kinds of coarse grains and white fine grains, and the specification of the barium carbonate is two kinds of analytical purity and spectral purity.
The silicon dioxide of the 1% germanium dioxide internal standard in the step (4) is prepared according to the following steps:
1.0000g of germanium dioxide is mixed into 100.0000g of white fine-grained silicon dioxide, and uniformly mixed on a ball mill for standby, wherein the process time is controlled as follows: 120-240 min.
The beneficial effects of the invention are as follows: (1) The spectrum carrier buffer prepared by the method can promote the oxidation, fluorination and sulfuration reactions of elements such as silver, boron, molybdenum, tin and the like in a sample within 30S, and the single-electrode carrier distillation method can improve the sensitivity of the element to be detected and the accuracy of an analysis result (2) the preparation method is simple and the raw materials are low in cost.
Drawings
FIG. 1 is a graph showing evaporation of each element to be tested when a spectral carrier buffer prepared in example 1 of the present invention reacts with a sample;
FIG. 2 shows the result of scanning electron microscopy of sintered bodies after reaction of the sample with the spectroscopic carrier buffer prepared in example 1 of the present invention.
Detailed Description
The invention will be further described with reference to the following detailed description of the drawings.
Example 1
The preparation method of the spectrum carrier buffer comprises the following specific steps:
(1) Firstly, accurately weighing potassium pyrosulfate (K) by an electronic balance 2 S 2 O 7 ) 4.0g was placed in an agate mortar and ground into a white fine powder.
(2) The crude Silica (SiO) was re-weighed in order 2 ) 0.6g and 1.0g of carbon powder (C) are respectively mixed with the potassium pyrosulfate in the step (1) and are uniformly ground.
(3) Another clean agate mortar was taken. 0.8g of sulfur powder and calcium carbonate (CaCO) were weighed by an electronic balance 3 ) 0.7g of iron oxide (Fe 2 O 3 ) 0.3g of polytetrafluoroethylene (not less than C) 2 F 2 And n) 0.4g are mixed well in a mortar and ground thoroughly.
(4) Analytically pure barium carbonate (BaCO) was weighed separately 3 ) 1.0g and spectrally pure barium carbonate (BaCO 3 ) 1.0g of Silica (SiO) containing 1% of germanium dioxide as an internal standard 2 ) 0.14g was mixed in a mortar; white fine-grained Silica (SiO) 2 ) 1.4g and 0.86g of sodium fluoride (NaF) are added to the mixtureThe mixture was thoroughly ground.
(5) Placing the above three ground mixtures in a clean agate tank, and weighing aluminum oxide (Al 2 O 3 ) 8.0g of powder is added into an agate tank together, and a proper amount of agate beads are put into the tank and are uniformly mixed on a ball mill.
(6) And (3) drying the final mixture obtained in the step (5) at 40-60 ℃ for 12 hours to obtain the spectrum carrier buffer.
And (3) in the steps (1), (2), (3), (4) and (5), the specifications of potassium pyrosulfate, carbon powder, sulfur powder, calcium carbonate, ferric oxide, polytetrafluoroethylene, sodium fluoride, aluminum oxide and germanium dioxide are analytically pure.
The silicon dioxide in the steps (2) and (4) is two kinds of coarse grains and white fine grains, and the specification of the barium carbonate is two kinds of analytical purity and spectral purity.
The silicon dioxide of the 1% germanium dioxide internal standard in the step (4) is prepared according to the following steps:
1.0000g of germanium dioxide is mixed into 100.0000g of white fine-grained silicon dioxide, and uniformly mixed on a ball mill for standby, wherein the process time is controlled as follows: 120-240 min.
When the prepared spectrum carrier buffer reacts with a sample, the evaporation curve of the element to be detected is shown in fig. 1: the evaporation trend changes of the elements are basically consistent, the 10 th evaporation peak value is reached, the evaporation is basically completed for 30 seconds, and the buffer can play a role in promoting the evaporation of the element to be detected.
Example 2
The preparation method of the spectrum carrier buffer comprises the following specific steps:
(1) Firstly, accurately weighing potassium pyrosulfate (K) by an electronic balance 2 S 2 O 7 ) 8.0g was placed in an agate mortar and ground into a white fine powder.
(2) The crude Silica (SiO) was re-weighed in order 2 ) 1.2g and 2.0g of carbon powder (C) are respectively mixed with the potassium pyrosulfate in the step (1) and are uniformly ground.
(3) Another clean agate mortar was taken. 1.6g of sulfur powder and calcium carbonate (CaCO) were weighed by an electronic balance 3 ) 1.4g, iron oxide (Fe 2 O 3 ) 0.6g of polytetrafluoroethylene (not less than C) 2 F 2 And n) 0.8g in a mortar and thoroughly ground.
(4) Analytically pure barium carbonate (BaCO) was weighed separately 3 ) 2.0g and spectrally pure barium carbonate (BaCO) 3 ) 2.0g of Silica (SiO) containing 1% of germanium dioxide as an internal standard 2 ) 0.28g was mixed in a mortar; white fine-grained Silica (SiO) 2 ) 2.8g and 1.72g of sodium fluoride (NaF) were added to the mixture and ground thoroughly.
(5) Placing the above three ground mixtures in a clean agate tank, and weighing aluminum oxide (Al 2 O 3 ) 16.0g of the powder is added into an agate tank together, and a proper amount of agate beads are put into the tank and mixed uniformly on a ball mill.
(6) And (3) drying the final mixture obtained in the step (5) at 40-60 ℃ for 12 hours to obtain the spectrum carrier buffer.
And (3) the specifications of potassium pyrosulfate, carbon powder, sulfur powder, calcium carbonate, ferric oxide, polytetrafluoroethylene, sodium fluoride, aluminum oxide and germanium dioxide in the steps (1) (2), (3), (4) and (5) are analytically pure.
The silicon dioxide in the steps (2) and (4) is two kinds of coarse grains and white fine grains, and the specification of the barium carbonate is two kinds of analytical purity and spectral purity.
The silicon dioxide of the 1% germanium dioxide internal standard in the step (4) is prepared according to the following steps:
1.0000g of germanium dioxide is mixed into 100.0000g of white fine-grained silicon dioxide, and uniformly mixed on a ball mill for standby, and the time is controlled as follows: 120-240 min.
After the above prepared spectral carrier buffer reacted with the sample, a large amount of matrix mixture remained as a complex salt solid solution as shown in sintered body Scanning Electron Microscope (SEM) fig. 2.
Example 3
The preparation method of the spectrum carrier buffer comprises the following specific steps:
(1) Firstly, accurately weighing potassium pyrosulfate (K) by an electronic balance 2 S 2 O 7 ) 12.0g of the mixture is put into agate for grindingIn a bowl, the mixture was ground into a white fine powder.
(2) The crude Silica (SiO) was re-weighed in order 2 ) 1.8g and 3.0g of carbon powder (C) are respectively mixed with the potassium pyrosulfate in the step (1) and are uniformly ground.
(3) Another clean agate mortar was taken. 2.4g of sulfur powder and calcium carbonate (CaCO) were weighed by an electronic balance 3 ) 2.1g, iron oxide (Fe 2 O 3 ) 0.9g of polytetrafluoroethylene (not less than C) 2 F 2 Not n) 1.2g are mixed in a mortar and ground thoroughly.
(4) Analytically pure barium carbonate (BaCO) was weighed separately 3 ) 3.0g and spectrally pure barium carbonate (BaCO) 3 ) 3.0g of Silica (SiO) containing 1% of germanium dioxide as an internal standard 2 ) 0.42g in a mortar; white fine-grained Silica (SiO) 2 ) 4.2g and 2.58g of sodium fluoride (NaF) were added to the mixture and ground thoroughly.
(5) Placing the above three ground mixtures in a clean agate tank, and weighing aluminum oxide (Al 2 O 3 ) 24.0g of the powder is added into an agate tank together, and a proper amount of agate beads are put into the agate tank to be uniformly mixed on a ball mill.
(6) And (3) drying the final mixed salt obtained in the step (5) at 40-60 ℃ for 12 hours to obtain the spectrum carrier buffer.
And (3) the specifications of potassium pyrosulfate, carbon powder, sulfur powder, calcium carbonate, ferric oxide, polytetrafluoroethylene, sodium fluoride, aluminum oxide and germanium dioxide in the steps (1) (2), (3), (4) and (5) are analytically pure.
The silicon dioxide in the steps (2) and (4) is two kinds of coarse grains and white fine grains, and the specification of the barium carbonate is two kinds of analytical purity and spectral purity.
The silicon dioxide of the 1% germanium dioxide internal standard in the step (4) is prepared according to the following steps:
1.0000g of germanium dioxide is mixed into 100.0000g of white fine-grained silicon dioxide, and uniformly mixed on a ball mill for standby, and the process control time is recommended as follows: 120-240 min.
Table 1 method precision test results of single electrode carrier distillation method
When the prepared spectrum carrier buffer method is tested, various national first-class geochemical standard substances are selected: stability tests were performed on aqueous sediment, soil and rock, and the relative standard deviation (RSD%) results for each element are shown in table 1.
Claims (5)
1. The preparation method of the atomic emission spectrum carrier distillation buffer is characterized by comprising the following specific steps:
(1) Weighing potassium pyrosulfate, placing in an agate mortar, and grinding into white fine powder;
(2) Weighing coarse silicon dioxide and carbon powder according to the sequence, respectively mixing with potassium pyrosulfate, and grinding uniformly;
(3) Weighing sulfur powder, calcium carbonate, ferric oxide and polytetrafluoroethylene in a clean agate mortar, uniformly mixing and fully grinding;
(4) Respectively weighing analytically pure barium carbonate and spectrally pure barium carbonate, adding GeO-containing material 2 Uniformly mixing silica of an internal standard in a mortar; weighing white fine-grained silicon dioxide and sodium fluoride, adding the white fine-grained silicon dioxide and the sodium fluoride into the mixture, and fully grinding;
(5) Placing the mixture obtained by grinding the three steps into a clean agate tank, adding the weighed aluminum oxide powder into the agate tank together, and placing agate beads into a ball mill to be uniformly mixed;
(6) And (3) drying the final mixture obtained in the step (5) at 40-60 ℃ for 12 hours to obtain the spectrum carrier buffer.
2. The method of preparing a spectroscopic carrier buffer of claim 1, wherein: the material consumption of each step is as follows:
in the step (1), 4.0 to 20.0g of potassium pyrosulfate;
in the step (2), the crude silicon dioxide is 0.6 to 3.0g, and the carbon powder is 1.0 to 5.0g;
in the step (3), 0.8 to 4.0g of sulfur powder, 0.7 to 3.5g of calcium carbonate, 0.3 to 1.5g of ferric oxide and 0.4 to 2.0g of polytetrafluoroethylene;
in the step (4), 1.0 to 5.0g of analytically pure barium carbonate, 1.0 to 5.0g of spectroscopically pure barium carbonate and GeO with the mass percent of 1 percent 2 0.7g of silica of an internal standard, 1.4-7.0 g of white fine silica and 0.86-4.3 g of sodium fluoride;
in the step (5), 8.0 to 40.0g of alumina is used.
3. The method of preparing a spectroscopic carrier buffer of claim 1, wherein: and (3) in the steps (1), (2), (3), (4) and (5), the specifications of potassium pyrosulfate, carbon powder, sulfur powder, calcium carbonate, ferric oxide, polytetrafluoroethylene, sodium fluoride, aluminum oxide and germanium dioxide are analytically pure.
4. The method of preparing a spectroscopic carrier buffer of claim 1, wherein: the content of GeO in the step (4) is 1% by mass 2 Silica of the internal standard is prepared according to the following steps:
mixing 1.0000g germanium dioxide into 100.0000g white fine silicon dioxide, and uniformly mixing on a ball mill for standby; the process time control is as follows: 120-240 min.
5. An atomic emission spectrometry supported distillation buffer, characterized in that it is obtainable by a process according to any one of claims 1 to 4.
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