CN113702410A - Analysis method for rapidly testing elements in nickel-containing waste residue - Google Patents
Analysis method for rapidly testing elements in nickel-containing waste residue Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000012360 testing method Methods 0.000 title claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 37
- 238000004458 analytical method Methods 0.000 title claims abstract description 36
- 239000002699 waste material Substances 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010561 standard procedure Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 229910052741 iridium Inorganic materials 0.000 claims description 8
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 229910052703 rhodium Inorganic materials 0.000 claims description 8
- 239000010948 rhodium Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 5
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical group [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000010944 silver (metal) Substances 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical group [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- WPEJSSRSFRWYJB-UHFFFAOYSA-K azanium;tetrachlorogold(1-) Chemical compound [NH4+].[Cl-].[Cl-].[Cl-].[Cl-].[Au+3] WPEJSSRSFRWYJB-UHFFFAOYSA-K 0.000 claims description 2
- 239000002893 slag Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 6
- 229910021538 borax Inorganic materials 0.000 description 5
- 239000004328 sodium tetraborate Substances 0.000 description 5
- 235000010339 sodium tetraborate Nutrition 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000009614 chemical analysis method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 101150003085 Pdcl gene Proteins 0.000 description 1
- 229910019029 PtCl4 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- -1 platinum ammonium chloride Chemical group 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/223—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 by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/312—Accessories, mechanical or electrical features powder preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/62—Specific applications or type of materials powders
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/635—Specific applications or type of materials fluids, granulates
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses an analysis method for rapidly testing each element in nickel-containing waste residue, which comprises the following steps: step one, setting analysis parameters of an instrument: 1) making a standard curve, 2) determining the element content of the standard sample by a national standard method to obtain the actual content X-valueiAnd 3) measuring the element content of the standard sample by an instrument and testing the content W by the instrumentiAnd 4) fitting a standard curve to obtain a correlation linear equation: x-i=ki Wi+ciAnd 5) setting analysis parameters of the instrument: adopting a geochem-extra method of an X-fluorescent alloy analyzer to establish a detection mode, wherein a factor parameter is modified to k-value in the detection modeiThe offset term parameter is modified to 10000ci(ii) a Step two, preparation of a sample: drying and grinding a sample to be detected, and placing the sample to be detected; step three, testing the sample: selecting the new detection mode in the instrument to treatAnd (5) detecting the sample. The invention has the advantages that: the method is simple to operate, high in analysis accuracy and short in detection whole process time.
Description
Technical Field
The invention relates to the technical field of element detection, in particular to an analysis method for rapidly testing each element in nickel-containing waste residue.
Background
The nickel anode mud is a product after electrolytic nickel is produced by hydrometallurgy, enriches a large amount of ores and concentrates, has high comprehensive recovery value, and can generate nickel hot filter residue in hot filter desulfurization, generate high-nickel waste residue in wet desulfurization, and generate waste residue after nickel removal when being comprehensively utilized, wherein the waste residue needs to test the element content in the waste residue to determine the enrichment condition of each element, thereby improving the recovery process.
The existing analysis method comprises the following steps: at present, the method for testing the elements is to test according to the test method recorded in the handbook for analyzing ores and nonferrous metals, wherein nickel, copper, iron and calcium can be analyzed by ICP or atomic absorption after the samples are dissolved, S is tested by a combustion neutralization method or a combustion iodometry method, Si samples are tested by a potassium fluosilicate titration method after alkali fusion, and gold, silver, platinum, palladium, rhodium and iridium are tested by the ICP or the atomic absorption method after the gold is enriched and separated by a fire test.
The prior method has the following defects: the existing method needs three different sample preparation methods to test different elements after a group of samples are tested by full indexes, the testing steps are complicated, and the testing time is long.
Disclosure of Invention
The invention aims to make up the defects and discloses an analysis method for rapidly testing each element in nickel-containing waste residue to the society, which has the advantages of simple operation, high analysis accuracy and short detection whole process time.
The technical scheme of the invention is realized as follows:
an analysis method for rapidly testing each element in nickel-containing waste residue comprises the following steps:
step one, setting analysis parameters of an instrument:
1) and (3) preparing a standard curve: preparing a standard curve by adopting a standard sample;
2) and (3) measuring the element content of the standard sample by a national standard method: the actual content of each element in the standard sample is tested by using the national standard method and is marked as XiI is the element type;
3) instrumental determination of elemental content of standard samples: the element content of the standard sample is measured by using an X-fluorescent alloy analyzer and is recorded as Wi；
4) Fitting of standard curve: measuring the actual content X in the third stepiAs ordinate, the content W was measured by an instrument in step fouriPerforming curve fitting as an abscissa to obtain a correlation linear equation: xi＝kiWi+ciWherein k isiIs the slope of a linear equation, ciIs the linear equation intercept;
5) setting analysis parameters of the instrument: adopting a geochem-extra method of an X-fluorescent alloy analyzer, and establishing a new detection mode, wherein in the new detection mode, a factor parameter is modified to be kiModifying the offset term parameter to 10000ci；
Step two, preparation of a sample: drying and grinding a sample to be detected, and placing the sample to be detected;
step three, testing the sample: and selecting the newly-built detection mode in the instrument to detect the sample to be detected.
The measures for further optimizing the technical scheme are as follows:
the elements comprise Ni, Cu, Fe, S, Si, Ca, Au, Ag, Pt, Pd, Rh and Ir.
As an improvement, in the first step, the standard curves are divided according to element content, wherein the standard curves are respectively established according to 0-1% of low content, 2-20% of medium content and 21-100% of high content.
In the second step, the drying temperature is 100-110 ℃.
As an improvement, in the second step, the sample to be tested is ground to a particle size of 120 meshes by using a grinder.
As an improvement, in the first step, the raw materials of the standard sample are selected from: nickel is selected from nickel sulfate and copper is selected from copper sulfate, iron is selected from ferric sulfate, sulfur is selected from elemental sulfur, silicon is selected from silicon dioxide, calcium is selected from calcium oxide, magnesium is selected from magnesium oxide, rhodium is selected from sodium hexachlororhodanide octadecahydrate, platinum is selected from ammonium platinate chloride, palladium is selected from sodium chloropalladate, iridium is selected from potassium iridate, gold is selected from ammonium chloroaurate, and silver is selected from silver chloride.
As an improvement, in the third step, before the sample to be tested is tested, the standard sample is tested, and the instrument is confirmed to be in a normal state.
Compared with the prior art, the invention has the advantages that:
according to the analysis method for rapidly testing each element in the nickel-containing waste residue, the parameter setting is carried out once on the X-fluorescent alloy analyzer, the parameter setting is not needed in the subsequent detection process, the pretreatment of the sample to be tested only needs to be carried out by drying and grinding, the method is very simple, the whole detection and analysis process of the sample to be tested can be completed only in 10-20 min, the detection time can be greatly saved, and the detection efficiency is improved.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
as shown in FIG. 1, an analysis method for rapidly testing each element in nickel-containing waste residue comprises the following steps:
step one, setting analysis parameters of an instrument:
1) and (3) preparing a standard curve: preparing a standard curve by adopting a standard sample;
the elements comprise Ni, Cu, Fe, S, Si, Ca, Au, Ag, Pt, Pd, Rh and Ir. Selection of standard sample raw materials: nickel is selected from nickel sulfate and copper is selected from copper sulfate, iron is selected from ferric sulfate, sulfur is selected from elemental sulfur, silicon is selected from silicon dioxide, calcium is selected from calcium oxide, magnesium is selected from magnesium oxide, corresponding salts are respectively selected from gold, silver, platinum, palladium, rhodium and iridium to be used as raw materials of a standard sample, and rhodium is selected from rhodiumRhodium sodium hexachloro-octadecahydrate (Na)3RhCl6·18H2O), platinum is selected from platinum ammonium chloride ((NH)4)2[PtCl4]) Palladium chloride sodium chloride (Na PdCl) for palladium separation4) The iridium is potassium iridate (K)2IrO3) The gold is sodium chloroaurate (NH)4AuCl4) Silver chloride (AgCl) is selected as silver. Standard stock samples: m g samples are weighed and mixed evenly for standby, and the analysis content of each element is carried out by using a national standard method, and the content is a reference standard value of each element in the standard stock sample. According to the concentration (respectively weighing 5g, 4g, 3g, 2.5g and 2g of standard stock samples in 5 groups of sample cups) of high content (respectively weighing 2g, 1.5g, 1.0g and 0.5g of standard stock samples in 5 groups of sample cups) and the concentration (respectively weighing 500mg, 200mg, 100mg, 50mg and 10mg of stock samples in 5 groups of sample cups), weighing by using one ten-thousandth of standard stock samples in the weighing balance process until the weight is accurate to 0.01mg, finally weighing 5g by using 120 meshes of borax and uniformly mixing the borax with the borax, sealing the borax in the sample cups and storing the borax in a dryer. And (3) testing: and testing by using an X-fluorescent alloy analyzer, selecting a geochem-extra method, selecting a user factor none, testing to obtain a corresponding coordinate point, and fitting to form a standard curve.
2) And (3) measuring the element content of the standard sample by a national standard method: the actual content of each element in the standard sample is tested by using the national standard method and is marked as XiAnd i is an element type.
3) Instrumental determination of elemental content of standard samples: the element content of the standard sample is measured by using an X-fluorescent alloy analyzer and is recorded as WiAnd i is an element type.
4) Fitting of standard curve: measuring the actual content X in the third stepiAs ordinate, the content W was measured by an instrument in step fouriPerforming curve fitting as an abscissa to obtain a correlation linear equation: xi＝kiWi+ciWherein k isiIs the slope of a linear equation, ciIs the linear equation intercept.
Because the coefficients of the related equations of the sample have differences in low content, medium content and high content, 3 standard curves of low content (0-1%), medium content (2-20%) and high content (21-100%) are prepared according to the content of elements, and the accuracy of the test can be improved.
5) Setting analysis parameters of the instrument: adopting a geochem-extra method of an X-fluorescent alloy analyzer to establish a detection mode, which is named as: ni11(H, M, L) mode, modifying the factor parameter of the mode to kiModifying the offset term parameter to 10000ci。
Step two, preparation of a sample: drying a sample to be detected at 100-110 ℃, grinding the sample to be detected to 120 meshes of particle size by using a grinder, and placing the sample to be detected; in this embodiment, 100g of the sample to be tested is weighed, dried at 105 ℃, and placed to be tested.
Step three, testing the sample: before testing the sample to be tested, testing the standard sample, confirming that the instrument is in a normal state, and selecting the newly-built detection mode in the instrument to detect the sample to be tested. The measured result shows that the mass percentage of certain element in the nickel-containing slag is Wi(%), the monitoring results are shown in the following table:
the analysis method for rapidly testing each element in the nickel-containing waste residue is convenient for sample treatment, only needs drying and grinding, directly detects the nickel-containing waste residue without resetting in the subsequent detection process after the parameters of a detection instrument (X-fluorescent alloy analyzer) are set for one time, only needs 10-20 min for each detection, and greatly improves the detection efficiency.
Several groups of samples were analyzed and compared by the analysis method of the present invention and the chemical analysis method, and the results of the analysis and comparison are shown in the following table:
sample 1: nickel anode slime: is a product after the electrolytic nickel is produced by hydrometallurgy;
sample 2: nickel hot slag filtration: hot filtering the anode mud to generate nickel hot filter residue;
sample 3: desulfurizing slag: slag is generated after the hot filter slag is desulfurized;
sample 4: removing nickel slag: slag is generated after the desulphurization slag is subjected to nickel removal.
And (3) analyzing test results: compared with a chemical analysis method, the analysis method has the advantages that the comparison results are within the error range, and the difference of partial results is slightly larger, but for the rapid detection method of production control, the deviation is within the acceptable range, the analysis method can provide the result with higher reliability within 10min-20, and compared with the chemical analysis method, the analysis method not only improves the analysis rate, but also can meet the process requirements, and has very high practical value.
According to the analysis method for rapidly testing each element in the nickel-containing waste residue, the parameter setting is not needed in the subsequent detection process by setting the parameter for one time for the X-fluorescent alloy analyzer, and the X-fluorescent alloy analyzer is calibrated by setting the parameter, so that the detection accuracy can be improved; before the sample to be detected is detected, the standard sample is tested, the instrument is confirmed to be in a normal state, and the detection accuracy can be further ensured.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (7)
1. An analysis method for rapidly testing each element in nickel-containing waste residue is characterized in that: the method comprises the following steps:
step one, setting analysis parameters of an instrument:
1) and (3) preparing a standard curve: preparing a standard curve by adopting a standard sample;
2) and (3) measuring the element content of the standard sample by a national standard method: the actual content of each element in the standard sample is tested by using the national standard method and is marked as XiI is the element type;
3) standard sample elementInstrumental determination of the content of elements: the element content of the standard sample is measured by using an X-fluorescent alloy analyzer and is recorded as Wi；
4) Fitting of standard curve: measuring the actual content X in the third stepiAs ordinate, the content W was measured by an instrument in step fouriPerforming curve fitting as an abscissa to obtain a correlation linear equation: xi＝ki Wi+ciWherein k isiIs the slope of a linear equation, ciIs the linear equation intercept;
5) setting analysis parameters of the instrument: adopting a geochem-extra method of an X-fluorescent alloy analyzer, and establishing a new detection mode, wherein in the new detection mode, a factor parameter is modified to be kiModifying the offset term parameter to 10000ci；
Step two, preparation of a sample: drying and grinding a sample to be detected, and placing the sample to be detected;
step three, testing the sample: and selecting the newly-built detection mode in the instrument to detect the sample to be detected.
2. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: the elements comprise Ni, Cu, Fe, S, Si, Ca, Au, Ag, Pt, Pd, Rh and Ir.
3. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: in the first step, the standard curves are divided according to element content, wherein the standard curves are respectively established according to 0-1% of low content, 2-20% of medium content and 21-100% of high content.
4. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: in the second step, the drying temperature is 100 ℃ to 110 ℃.
5. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: in the second step, the sample to be detected is ground to 120 meshes by a grinder.
6. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: in the first step, the raw materials of the standard sample are selected as follows: nickel is selected from nickel sulfate and copper is selected from copper sulfate, iron is selected from ferric sulfate, sulfur is selected from elemental sulfur, silicon is selected from silicon dioxide, calcium is selected from calcium oxide, magnesium is selected from magnesium oxide, rhodium is selected from sodium hexachlororhodanide octadecahydrate, platinum is selected from ammonium platinate chloride, palladium is selected from sodium chloropalladate, iridium is selected from potassium iridate, gold is selected from ammonium chloroaurate, and silver is selected from silver chloride.
7. The analytical method for rapidly testing various elements in the nickel-containing waste residue as claimed in claim 1, which is characterized in that: and step three, before testing the sample to be tested, testing the standard sample and confirming that the instrument is in a normal state.
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| CN104897710A (en) * | 2015-06-19 | 2015-09-09 | 金川集团股份有限公司 | Analyzing method for rapid and simultaneous determination of Ni, Cu, Fe, S, Pb, Zn, As, Sb, Bi and SiO2 in copper matte |
| CN106248707A (en) * | 2016-07-21 | 2016-12-21 | 金川集团股份有限公司 | Ni, Cu, Fe, S, CaO, MgO, SiO in a kind of quickly translocation flash smelting slag2, the analysis method of Pb, Zn, As, Sb, Bi |
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| CN109387532A (en) * | 2017-08-02 | 2019-02-26 | 张家港浦项不锈钢有限公司 | The method of the cold milling of intermediate frequency MTG YBCO bulk-X-Ray fluorescence spectrum method for measuring nickel |
| CN113311015A (en) * | 2021-06-11 | 2021-08-27 | 湖北亿纬动力有限公司 | Method for analyzing content of main elements in nickel cobalt lithium manganate positive electrode material |
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| CN104897710A (en) * | 2015-06-19 | 2015-09-09 | 金川集团股份有限公司 | Analyzing method for rapid and simultaneous determination of Ni, Cu, Fe, S, Pb, Zn, As, Sb, Bi and SiO2 in copper matte |
| CN106248707A (en) * | 2016-07-21 | 2016-12-21 | 金川集团股份有限公司 | Ni, Cu, Fe, S, CaO, MgO, SiO in a kind of quickly translocation flash smelting slag2, the analysis method of Pb, Zn, As, Sb, Bi |
| CN107340276A (en) * | 2017-07-06 | 2017-11-10 | 钢研纳克检测技术有限公司 | A kind of method of multiple element content in quick measure rare earth metal/alloy |
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