CN116593345A - Quantitative detection method for gold content in alloy containing non-gold noble metal - Google Patents
Quantitative detection method for gold content in alloy containing non-gold noble metal Download PDFInfo
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 239000010931 gold Substances 0.000 title claims abstract description 166
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 162
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 113
- 239000000956 alloy Substances 0.000 title claims abstract description 113
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 14
- 238000001514 detection method Methods 0.000 title abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 58
- 239000000706 filtrate Substances 0.000 claims abstract description 50
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 50
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 49
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000012360 testing method Methods 0.000 claims abstract description 37
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims abstract description 34
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 29
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052762 osmium Inorganic materials 0.000 claims abstract description 28
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 26
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 25
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 24
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 24
- 239000010948 rhodium Substances 0.000 claims abstract description 24
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 24
- 238000012937 correction Methods 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 12
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- 238000004090 dissolution Methods 0.000 claims description 11
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical group [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910052709 silver Inorganic materials 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011133 lead Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- NTVYFDOMBHOLGP-UHFFFAOYSA-N gold nitric acid Chemical compound [Au].O[N+]([O-])=O NTVYFDOMBHOLGP-UHFFFAOYSA-N 0.000 description 1
- ZVUZTTDXWACDHD-UHFFFAOYSA-N gold(3+);trinitrate Chemical compound [Au+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O ZVUZTTDXWACDHD-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000011410 subtraction method Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The application discloses a quantitative detection method for gold content in alloy containing non-gold noble metal, and belongs to the technical field of noble metal determination. The method comprises the following steps: (1) Weight is M 0 Dissolving the alloy to be detected in aqua regia solution or hydrochloric acid solution containing chlorate, and collecting filtrate A; (2) Reducing the filtrate A by adopting a reducing agent, and separating solids to obtain filtrate B; (3) Melting the obtained solid at high temperature to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 Weight of sample to be tested sample gold paper is prepared by fire test gold weight method, and weight M of sample gold paper is recorded 2 And calculate the average value of correction values of the standard sample gold coil(4) Dissolving the sample gold coil with aqua regia to obtain solution, and calculating platinum, palladium, rhodium, ruthenium, iridium and osmium in the solutionM is the total weight of (2) 4 The method comprises the steps of carrying out a first treatment on the surface of the (5) calculating the gold content in the alloy. The method can eliminate the influence of platinum, palladium, rhodium, ruthenium, iridium and osmium elements on the detection result of the gold content in the alloy, so that the gold content in the alloy can be quantitatively obtained.
Description
Technical Field
The application relates to a quantitative detection method for gold content in alloy containing non-gold noble metal, belonging to the technical field of noble metal determination.
Background
The detection methods used in the current detection of the alloy mainly use three methods of GB/T15249.1-2009, GB/T9288-2019 and GB/T11066.1-2008, but all three methods are not suitable for detecting the alloy containing noble metals such as platinum, palladium, rhodium, ruthenium, iridium and osmium.
The above elements are not oxidized and separated from gold and silver in the high temperature molten ash blowing process in the detection process, so that the elements cannot be separated from gold in the subsequent nitric acid gold separation process, so that samples containing the elements often have macroscopic 'unknown black substances' on gold rolls prepared by detection, the detection result of the alloy is inaccurate, and the conventional fire-test gold detection weight method is not suitable for the detection of the samples.
The inventor finds that elements such as iridium are not uniformly distributed in the alloy after being melted at high temperature, but are more intensively distributed on one side of the alloy after cooling and solidification through long-term detection analysis, so that samples prepared by a common drilling method and the like lose representativeness when facing samples containing the elements, and subsequent detection results lose significance, and no suitable method for accurately detecting the gold content in the alloy containing non-gold noble metals insoluble in nitric acid exists at present.
Disclosure of Invention
In order to solve the problems, the method is provided for quantitatively detecting the gold content in the alloy containing non-gold noble metals, the method is characterized in that the alloy to be detected is placed in aqua regia or hydrochloric acid solution containing chlorate to be dissolved, so that the separation of most iridium and osmium elements and gold elements can be realized, then gold coil is dissolved in the aqua regia again, the total content of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution is measured, the weight of the gold coil only containing gold and silver can be obtained after deduction, and the correction average value of the standard sample gold coil is obtained by a fire test gold weight method to be corrected, so that the gold content in the alloy can be quantitatively obtained.
The application provides a method for detecting gold content in alloy containing non-gold noble metal, which comprises the following steps:
(1) Weight is M 0 Dissolving the alloy to be detected in aqua regia solution or hydrochloric acid solution containing chlorate, and separating insoluble matters to obtain filtrate A;
(2) Reducing the filtrate A by adopting a reducing agent, and separating solids to obtain filtrate B;
(3) Melting the obtained solid at high temperature to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 The weight of the sample to be tested is prepared into a sample gold volume by a fire test gold weight method, and the weight M of the sample gold volume is recorded 2 And calculate the average value of correction values of the standard sample gold coil
(4) Dissolving the sample gold coil in the step (3) by aqua regia to obtain a solution, testing the content of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution, and calculating the total weight M of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution 4 ；
(5) The gold content in the alloy was calculated according to the following formula:
the four elements of platinum, palladium, rhodium and ruthenium can be dissolved in aqua regia or hydrochloric acid solution containing chlorate, but the four elements cannot be thoroughly separated from gold in the gold nitrate process when analyzed by a fire gold test method, so that the detection result is higher. The iridium and osmium are extremely small in quantity and dissolved in aqua regia or hydrochloric acid solution containing chlorate, so that gold elements in the alloy are all dissolved in gold-containing filtrate, and the primary separation of the iridium and osmium and the gold elements can be realized in the step (1); when the reducing agent in the step (2) reduces the filtrate A, gold elements are reduced into gold powder, platinum, palladium, rhodium and ruthenium, and a very small amount of iridium and osmium dissolved in aqua regia or hydrochloric acid solution containing chlorate are reduced and mixed in the gold powder, but at this time, the dispersion of the elements in the gold powder is not uniform, so that the gold powder solid is melted at high temperature in the step (3) to obtain a sample to be detected, and at this time, the elements in the sample to be detected are uniformly distributed, and the obtained sample gold coil does not contain 'unknown black substances', so that the accuracy of a final calculation result can be improved; and (4) dissolving the sample gold coil in aqua regia again, so that all the platinum, palladium, rhodium, ruthenium, and very little iridium and osmium contained in the sample gold coil are dissolved in the aqua regia, the total weight of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution is calculated, the gold coil mass only containing gold and silver is obtained after deduction, and the standard sample gold coil is adopted to calculate and obtain the correction value average value of the standard sample gold coil for correction, so that the gold powder content in the alloy can be calculated.
Optionally, the method further comprises the step of measuring and calculating the weight of gold in the filtrate B of the step (2):
determining the gold content in the filtrate B in the step (2), and calculating the weight M of gold contained in the filtrate B according to the volume of the filtrate B 3 The gold content in the alloy is calculated according to the following formula:
in the step (2), the reducing agent is adopted to reduce the filtrate A to obtain a solid containing gold powder, and the residual gold element in the filtrate B is very small, so that the gold content in the filtrate B is calculated, and all gold elements contained in the alloy can be counted, so that the accuracy of the detection method is further improved.
Optionally, determining the gold content in the filtrate of step (2) using an ICP spectrometer or an atomic absorption spectrometer.
When the Siemens flight ICP6300 or 6500 spectrometer is adopted, the test wavelength is 242.795nm, the equipment use temperature is 18-23 ℃, the RF power of ICP is 1150w, the peristaltic pump rotating speed is 50r/min, and the carrier gas and auxiliary gas flow rate is 0.5L/min; when an atomic absorption spectrometer is used, the measurement is carried out with a gold hollow cathode lamp at a wavelength of 242.8 nm.
Optionally, in the step (1), the alloy to be measured is powder or flake, the particle size of the powder is 150-180 meshes, and the thickness of the flake is 0.05-0.1mm.
The particle size of the powder and the thickness of the thin sheet can increase the dissolution rate of gold element in the alloy to be detected in aqua regia or hydrochloric acid solution containing chlorate, shorten the dissolution time of the alloy, and increase the dissolution rate of the gold element, and meanwhile, the iridium and osmium can be dissolved in a small amount, but on the premise of shortening the overall dissolution time of the alloy, the total amount of the iridium and osmium doped in the filtrate A is still lower than the amount of the element obtained by dissolving the whole alloy, so that the primary separation degree of the two elements and the gold element is further improved.
Optionally, in the step (1), the concentration of the hydrochloric acid in the hydrochloric acid solution containing chlorate is 25% -30%, the concentration of the chlorate in the hydrochloric acid solution containing chlorate is potassium chlorate or sodium chlorate, the weight ratio of the potassium chlorate to the alloy to be detected is 0.5-0.7:1, and the weight ratio of the sodium chlorate to the alloy to be detected is 0.5-0.7:1.
The hydrochloric acid solution containing chlorate can quickly dissolve gold elements, and the substances and the concentration are arranged on the basis of ensuring that the gold elements in the alloy are quickly dissolved, so that the dissolving amount of platinum, palladium, rhodium, ruthenium, iridium and osmium is reduced, and the accuracy and precision of a detection result are improved.
Optionally, in the step (2), the reducing agent is hydrazine hydrate, excessive hydrazine hydrate is added, and the reducing agent is stirred for 50-80min at 20-30 ℃.
The arrangement can realize rapid reduction of gold powder, and reduce the residual quantity of gold elements in the filtrate B, so that detection errors are reduced, and the industrial detection needs can be met even on the basis that the gold elements in the filtrate B are not calculated.
Preferably, after the hydrazine hydrate is adopted for reduction, the solution is heated to boiling and then solids are separated, and the heating process can promote the reduced solids in the filtrate A to be polymerized rapidly, so that the filtrate A is clarified, and the solid separation efficiency is improved.
Optionally, measuring the content of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution in the step (4) by using an ICP spectrometer or an atomic absorption spectrometer.
When an ICP spectrometer is used, the test wavelength is 242.795nm; the test wavelength of the platinum element is 265.945nm, the test wavelength of the palladium element is 340.458nm, the test wavelength of the rhodium element is 343.489nm, the test wavelength of the ruthenium element is 267.876nm, the test wavelength of the iridium element is 215.268nm, and the test wavelength of the osmium element is 225.585nm.
Optionally, in the step (3), the solid is placed at a high temperature of 1100-1300 ℃ and melted for 5-10min to obtain the sample to be tested. By melting under the above conditions, the powder with uneven component content can be changed into a uniform sample, and organic matters possibly existing in the powder can be removed at high temperature, thereby ensuring the accuracy of the detection result.
Optionally, the saidThe calculation formula of (2) is as follows:
wherein M is 5 To correct the weight of the gold paper obtained by Jin Biaoyang through the fire test gold weight method, the unit is mg, M 6 The weight of the correction Jin Biaoyang which is weighed before the corresponding M5 gold coil passes through the fire test gold weight method process is measured, the unit is mg, and D is the mass fraction of gold in the standard sample.
Optionally, the volume weight ratio of the alloy to be detected to the aqua regia solution is 1: (6-10), wherein the unit is g/ml, the weight ratio of aqua regia to solvent water in the aqua regia solution is 1:1, and the dissolution temperature is 50-90 ℃;
the volume weight ratio of the alloy to be detected to the hydrochloric acid solution containing chlorate is 1: (6-10), the unit is g/ml, and the dissolution temperature is 85-90 ℃.
The beneficial effects of the application include, but are not limited to:
1. according to the quantitative detection method provided by the application, 6 elements influencing the result of the gravimetric method are separated and subtracted, so that the accuracy and precision of the detection result are good, and the requirements of repeatability and reproducibility of the alloy content test method in related countries and industry standard detection methods are met.
2. According to the quantitative detection method disclosed by the application, the alloy to be detected is dissolved twice, the influence of 'platinum, palladium, rhodium, ruthenium, iridium and osmium' elements on the detection result of the gold content in the alloy is eliminated, so that the representativeness of a sample used in detection is ensured, the detection capability of the alloy with complex components is greatly improved, and the method has a good guiding effect on raw material purchase and trade settlement of the sample.
3. According to the quantitative detection method provided by the application, the residual gold elements in the filtrate B are calculated, so that all gold elements contained in the alloy can be counted, and the accuracy of the detection method provided by the application is further improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a diagram of a sample to be tested obtained by cooling after the high-temperature melting of the solid in the step (3) is completed;
fig. 2 is a diagram of a process for washing an alloy coil.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless otherwise indicated, all starting materials in the examples of the present application were purchased commercially.
The ICP spectrometer used in the application has the model numbers of ICP6500 and ICP6300, and the manufacturer is Sieimer's Feier;
the model of the atomic absorption spectrometer is ICE3300, and the manufacturer is Sieimer's Feishier.
The average value of correction values to the standard sample gold coil is used in the calculation formula of the following embodimentThe method comprises the steps of supplementing a certain amount of silver to a sample, wrapping the sample with a certain amount of lead, putting the sample into a cupel preheated in a muffle furnace until ash blowing is completed, hammering the obtained gold and silver particles into sheets, grinding the sheets into sheets on a sheet grinding machine, putting the sheets into nitric acid for silver removal, and washing, drying and annealing at high temperature the gold coil obtained after silver removal by the nitric acid twice. The calculation formula is as follows: />Wherein M is 5 To correct the weight of the gold paper obtained by Jin Biaoyang through the fire test gold weight method, the unit is mg, M 6 The weight of the correction Jin Biaoyang which is weighed before the corresponding M5 gold coil passes through the fire test gold weight method flow is measured, the unit is mg, and the D is the mass fraction of gold in the standard sample, and the weight percentage is 99.99 percent.
Example 1
The embodiment relates to a method for detecting gold content in alloy containing non-gold noble metal, which comprises the following steps:
(1) Weight is M 0 The alloy to be measured is dissolved in aqua regia solution, the dissolution temperature is 90 ℃, and the volume weight ratio of the alloy to be measured to the aqua regia solution is 1:6, the unit is g/ml, the weight ratio of aqua regia to solvent water in the aqua regia solution is 1:1, wherein the particle size of the alloy to be detected is 150 meshes, and insoluble matters are separated to obtain filtrate A;
(2) Reducing the filtrate A by adopting hydrazine hydrate, adding excessive hydrazine hydrate, stirring and reducing for 60min at 25 ℃, heating to boiling, and separating solids to obtain filtrate B;
(3) Melting the obtained solid at 1200deg.C for 7min to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 Weight of sample to be tested sample gold paper is prepared by fire test gold weight method, and weight M of sample gold paper is recorded 2 And calculate the average value of correction values of the standard sample gold coil
(4) Dissolving the sample gold coil in the step (3) by aqua regia to obtain a solution, testing the contents of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution by adopting an ICP spectrometer, and calculating the total weight M of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution 4 ；
(5) The gold content in the alloy was calculated according to the following formula:
the above example 1 was used to test the alloy No. 1 and the alloy No. 2, respectively, and the results are shown in table 1, the gold coil obtained by the procedure of example 1 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was made for the alloy No. 1 and the alloy No. 2.
Table 1 example 1
Example 2
The embodiment relates to a method for detecting gold content in alloy containing non-gold noble metal, which comprises the following steps:
(1) Weight is M 0 The alloy to be measured is dissolved in hydrochloric acid solution containing potassium chlorate, the dissolution temperature is 85 ℃, and the volume weight ratio of the alloy to be measured to the hydrochloric acid solution containing potassium chlorate is 1:6, separating insoluble matters to obtain filtrate A, wherein the unit is g/ml, the particle size of the alloy to be detected is 180 meshes, the concentration of hydrochloric acid is 25%, and the weight ratio of potassium chlorate to the alloy to be detected is 0.6:1;
(2) Reducing the filtrate A by adopting hydrazine hydrate, adding excessive hydrazine hydrate, stirring and reducing for 50min at 30 ℃, heating to boiling, and separating solids to obtain filtrate B;
(3) Melting the obtained solid at 1300 deg.C for 5min to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 Weight of the sample to be tested is prepared by a fire test weight methodSample gold roll, weight M of sample gold roll is recorded 2 And calculate the average value of correction values of the standard sample gold coil
(4) Dissolving the sample gold coil in the step (3) by aqua regia to obtain a solution, testing the contents of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution by adopting an ICP spectrometer, and calculating the total weight M of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution 4 ；
(5) The gold content in the alloy was calculated according to the following formula:
the above-mentioned example 2 was used to test the alloy No. 1 and alloy No. 2, respectively, and the results are shown in table 2, in which the gold coil obtained by the procedure of example 1 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold were made for each of the alloy No. 1 and alloy No. 2.
Table 2 example 2
Example 3
The embodiment relates to a method for detecting gold content in alloy containing non-gold noble metal, which comprises the following steps:
(1) Weight is M 0 The alloy to be measured is dissolved in aqua regia solution, the dissolution temperature is 50 ℃, and the volume weight ratio of the alloy to be measured to the aqua regia solution is 1:10, wherein the unit is g/ml, the weight ratio of aqua regia to solvent water in the aqua regia solution is 1:1, the alloy to be detected is in a flake shape, the thickness of the flake is 0.05mm, and insoluble matters are separated to obtain filtrate A;
(2) Reducing the filtrate A by adopting hydrazine hydrate, adding excessive hydrazine hydrate, stirring and reducing for 80min at 20 ℃, and separating solids to obtain filtrate B;
(3) Melting the obtained solid at 1100 deg.C for 10min to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 Weight of sample to be tested sample gold paper is prepared by fire test gold weight method, and weight M of sample gold paper is recorded 2 And calculate the average value of correction values of the standard sample gold coil
(4) Dissolving the sample gold coil in the step (3) by aqua regia to obtain a solution, testing the contents of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution by adopting an ICP spectrometer, and calculating the total weight M of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution 4 ；
(5) The gold content in the alloy was calculated according to the following formula:
the above-mentioned example 3 was used to test the alloy No. 1 and alloy No. 2, respectively, and the results are shown in table 1, in which the gold coil obtained by the procedure of example 3 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was produced for each of the alloy No. 1 and alloy No. 2.
TABLE 3 example 3
Example 4
This example further comprises the step of measuring and calculating the weight of gold in filtrate B of step (2) on the basis of example 1:
measuring the gold content in the filtrate B in the step (2) by adopting an ICP spectrometer, and calculating the weight M of gold in the filtrate B according to the volume of the filtrate B 3 The gold content in the alloy was calculated according to the following formula:
the above-mentioned example 4 was used to test the alloy No. 1 and alloy No. 2, respectively, and the results are shown in table 1, in which the gold coil obtained by the procedure of example 4 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was produced for each of the alloy No. 1 and alloy No. 2.
Table 4 example 4
Example 5
This example differs from example 1 in that the filtrate a was reduced with sulfurous acid, excess hydrazine hydrate was added, and the mixture was stirred and reduced at 25 ℃ for 60min, the remaining steps and test formulas being the same as in example 1.
The above-mentioned example 5 was used to test the alloy No. 1 and alloy No. 2, respectively, and the results are shown in table 1, in which the gold coil obtained by the procedure of example 5 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was produced for each of the alloy No. 1 and alloy No. 2.
TABLE 5 example 5
Example 6
This example further comprises the step of measuring and calculating the weight of gold in filtrate B of step (2) on the basis of example 5:
measuring the gold content in the filtrate B in the step (2) by adopting an ICP spectrometer, and calculating the weight M of gold in the filtrate B according to the volume of the filtrate B 3 The gold content in the alloy was calculated according to the following formula:
the above-mentioned example 6 was used to test the alloy No. 1 and alloy No. 2, respectively, and the results are shown in table 1, in which the gold coil obtained by the procedure of example 6 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was produced for each of the alloy No. 1 and alloy No. 2.
TABLE 6 example 6
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Comparative example 1
The difference between this comparative example and example 1 is that step (4) was not performed, and the gold content in the alloy was calculated according to the following formula:
the above comparative example 1 was used to test the alloy No. 1 and the alloy No. 2, respectively, and the results are shown in table 7, in which the gold coil obtained by the procedure of comparative example 1 did not show an unclear black material, wherein 1# -8# represents a parallel experiment, and only 4 standard gold was produced for each of the alloy No. 1 and the alloy No. 2.
Table 7 comparative example 1
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Comparative example 2
The comparative example adopts a fire test gold weight method to measure the gold content in alloy, and the specific method comprises the following steps: taking M 1 The alloy sample is added with silver according to the proportion of gold to silver of 1:2.5, is wrapped by lead, is subjected to ash blowing at 960 ℃, and gold and silver alloy grains obtained after ash blowing are crushed into pieces, annealed, rolled and annealed to prepare an alloy coil. Separating gold from the alloy coil in nitric acid twice to obtain gold coil, washing, stoving, annealing and weighing to obtain gold coil with final mass M 2 Simultaneously calculating the correction average value of the standard sample gold coilThe gold content of the sample was calculated. And then calculating the gold content in the alloy according to the following calculation formula:
the above comparative example 2 was used to detect the alloy No. 1 and the alloy No. 2, respectively, and the results are shown in table 8, in which the gold coil obtained by the procedure of comparative example 2 showed an unclear black material, wherein 1# -8# represents a parallel experiment, and the alloy No. 1 and the alloy No. 2 were each only made 4 standard gold.
Table 8 comparative example 2
Comparative example 3
In the comparative example, the alloy to be measured is dissolved in aqua regia solution, the volume is fixed at 25ml, and the volume weight ratio of the alloy to be measured to the aqua regia solution is 1:6, the unit is g/ml, the weight ratio of aqua regia to solvent water in the aqua regia solution is 1:1, wherein the grain diameter of the alloy to be detected is 150 meshes, insoluble substances are separated to obtain filtrate A, the contents of 13 elements of silver, iron, copper, lead, antimony, bismuth, platinum, palladium, nickel, chromium, magnesium, manganese and tin in the filtrate A are measured by ICP, the total content of the 13 elements is calculated, the gold content is calculated by a subtraction method, and the total content of omega (Au) =100-13 elements is calculated.
The results of the respective tests on the alloy No. 1 and the alloy No. 2 were shown in Table 9, in which 1# -8# represents a parallel experiment.
Table 9 comparative example 3
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According to the data, the gold content in the alloy can be quantitatively obtained, the repeatability and reproducibility of the detection result meet the requirements of GB/T15249.1-2009 method, the influence of 'platinum, palladium, rhodium, ruthenium, iridium and osmium' elements on the gold content detection result in the alloy is eliminated, the detection capability of the alloy with complex components is greatly improved, and the method can be used for guiding the raw material acquisition, trade settlement and other aspects of the sample.
The above description is only an example of the present application, and the scope of the present application is not limited to the specific examples, but is defined by the claims of the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A method for quantitatively detecting gold content in an alloy containing a non-gold noble metal, comprising the steps of:
(1) Weight is M 0 Dissolving the alloy to be detected in aqua regia solution or hydrochloric acid solution containing chlorate, separating insoluble matters, and collecting filtrate A;
(2) Reducing the filtrate A by adopting a reducing agent, and separating solids to obtain filtrate B;
(3) Melting the obtained solid at high temperature to obtain a solid with weight of M 0 ' sample to be measured, weighing M 1 The weight of the sample to be tested is prepared into a sample gold volume by a fire test gold weight method, and the weight M of the sample gold volume is recorded 2 Calculating the average value delta m of correction values of the standard sample gold coil;
(4) Dissolving the sample gold coil in the step (3) by aqua regia to obtain a solution, testing the content of platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution, and calculating the total weight M of the platinum, palladium, rhodium, ruthenium, iridium and osmium in the solution 4 ；
(5) The gold content in the alloy was calculated according to the following formula:
ω(Au)＝[(M 2 -M 4 -Δm)/M 1 ]×(M 0 ’/M 0 )×100。
2. the method of claim 1, further comprising the step of determining and calculating the weight of gold in filtrate B of step (2):
determining the gold content in the filtrate B in the step (2), and calculating the weight M of gold contained in the filtrate B according to the volume of the filtrate B 3 The gold content in the alloy was calculated according to the following formula:
ω(Au)＝[((M 2 +M 3 -M 4 -Δm)/M 1 ]×(M 0 ’/M 0 )×100。
3. the method of claim 2, wherein the gold content of the filtrate of step (2) is determined using an ICP spectrometer or an atomic absorption spectrometer.
4. The method according to claim 1, wherein in the step (1), the alloy to be measured is a powder or a flake, the particle size of the powder is 150 to 180 mesh, and the thickness of the flake is 0.05 to 0.1mm.
5. The method of claim 1, wherein in step (1), the concentration of hydrochloric acid in the chlorate-containing hydrochloric acid solution is 25% to 30%;
in the hydrochloric acid solution containing chlorate, the chlorate is potassium chlorate or sodium chlorate, the weight ratio of the potassium chlorate to the alloy to be detected is 0.5-0.7:1, and the weight ratio of the sodium chlorate to the alloy to be detected is 0.5-0.7:1.
6. The method according to claim 1, wherein in the step (2), the reducing agent is hydrazine hydrate, an excessive amount of hydrazine hydrate is added, and the mixture is stirred and reduced at 20-30 ℃ for 50-80min.
7. The method of claim 1, wherein the content of platinum, palladium, rhodium, ruthenium, iridium, osmium in the solution of step (4) is measured using an ICP spectrometer or an atomic absorption spectrometer.
8. The method according to claim x, wherein in step (3), the solid is subjected to high temperature melting at 1100-1300 ℃ for 5-10min to obtain the sample to be tested.
9. The method according to claim 1, wherein the Δm is calculated by the formula:
Δm＝M 5 -M 6 x D, where M 5 To correct the weight of the gold paper obtained by Jin Biaoyang through the fire test gold weight method, the unit is mg, M 6 The weight of the correction Jin Biaoyang which is weighed before the corresponding M5 gold coil passes through the fire test gold weight method process is measured, the unit is mg, and D is the mass fraction of gold in the standard sample.
10. The method according to claim 1, wherein the volume to weight ratio of the alloy to be measured to the aqua regia solution is 1: (6-10), wherein the unit is g/ml, the weight ratio of aqua regia to solvent water in the aqua regia solution is 1:1, and the dissolution temperature is 50-90 ℃;
the volume weight ratio of the alloy to be detected to the hydrochloric acid solution containing chlorate is 1: (6-10), the unit is g/ml, and the dissolution temperature is 85-90 ℃.
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