CN116577233A - Method for quantitatively detecting gold content in gold cyanide mud - Google Patents
Method for quantitatively detecting gold content in gold cyanide mud Download PDFInfo
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- 239000010931 gold Substances 0.000 title claims abstract description 171
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 162
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 46
- 229910052709 silver Inorganic materials 0.000 claims abstract description 53
- 239000004332 silver Substances 0.000 claims abstract description 53
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 50
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052802 copper Inorganic materials 0.000 claims abstract description 46
- 239000010949 copper Substances 0.000 claims abstract description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000007664 blowing Methods 0.000 claims abstract description 25
- 239000011888 foil Substances 0.000 claims abstract description 20
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 17
- 229910001316 Ag alloy Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 claims abstract description 14
- MXZVHYUSLJAVOE-UHFFFAOYSA-N gold(3+);tricyanide Chemical compound [Au+3].N#[C-].N#[C-].N#[C-] MXZVHYUSLJAVOE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 33
- 229910017604 nitric acid Inorganic materials 0.000 claims description 33
- 238000000926 separation method Methods 0.000 claims description 20
- 239000010802 sludge Substances 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 229910001020 Au alloy Inorganic materials 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 239000010970 precious metal Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 32
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229910000510 noble metal Inorganic materials 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 24
- 238000002474 experimental method Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 8
- 238000010998 test method Methods 0.000 description 6
- 239000011246 composite particle Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000010009 beating Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
Abstract
The application discloses a method for quantitatively detecting gold content in cyanide gold mud, and belongs to the technical field of noble metal determination. The detection method comprises the following steps: (1) Estimating the content of gold, silver, copper and nickel in the cyanide gold mud sample; (2) preparing a sample: weighing a gold cyanide mud sample, putting the gold cyanide mud sample into a lead foil, and adding lead and silver to obtain a sample, wherein the adding amount of the lead is 40-60 times of the estimated copper weight, and the weight ratio of the gold to the silver in the sample is 1: (2.5-15); (3) preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the detection sample, adding copper with the same weight ratio as the detection sample, and putting the mixture into a lead foil; (4) And blowing the oxygen-enriched ash of the sample and the standard sample in a high-temperature molten state to obtain gold-silver alloy particles respectively, separating gold to obtain sample gold and standard sample gold, and calculating the gold content in the gold cyanide mud sample. The detection method has high accuracy and precision, reduces detection cost and detection time, and provides reliable data guidance for the production process of gold cyanide mud.
Description
Technical Field
The application relates to a method for quantitatively detecting gold content in cyanide gold mud, and belongs to the technical field of noble metal determination.
Background
The gold cyanide mud can be obtained by zinc powder replacement, and the gold content in the gold cyanide mud prepared by the method is influenced by a plurality of factors, so that the range of the gold content in a sample is greatly fluctuated, the gold content in the gold cyanide mud is accurately measured, and the preparation process of the gold cyanide mud can be fed back, so that the cyanidation leaching production process is conveniently optimized, and more accurate stock quantity of gold can be conveniently obtained during inventory.
At present, no standard detection method for detecting the gold content in cyanide gold mud exists, and many enterprises detect the gold by a fire test method for detecting the gold content in GB/T7739.1-2019 gold concentrate. However, when the sample containing high gold and silver content is faced, the effect of capturing gold and silver is affected by lead, the detection result is low, and if the sample contains high content of copper and other impurities, the detection result is affected. Therefore, under the test method, the gold content of the gold is usually measured by performing secondary gold test and tertiary gold test, but the test steps of the secondary gold test and the tertiary gold test are complicated, so that the test time is long, the test cost is increased, the gold content in partial cyanide gold mud is higher, the gold content can be detected by referring to the fire gold test method of alloy gold, but the gold content in most cyanide gold mud is in the range of 10% -20%, even lower than 5%, and the gold-silver ratio is far higher than 1:2.5, so that the fire gold test method of alloy gold is not fully applicable, and a method capable of rapidly and quantitatively detecting the gold content in cyanide gold mud is needed.
Disclosure of Invention
In order to solve the problems, the method for quantitatively detecting the gold content in the gold cyanide mud is provided, the detection method can rapidly finish quantitative detection of the gold content in the gold cyanide mud, the accuracy and precision of a detection result are high, the detection cost and the detection time are reduced, and reliable data guidance is provided for the gold cyanide mud leaching production process.
The application provides a method for quantitatively detecting gold content in cyanide gold mud, which comprises the following steps:
(1) Estimating the content of gold, silver and copper in the cyanide gold mud sample;
(2) Preparing a sample: weighing a gold cyanide mud sample, putting the gold cyanide mud sample into a lead foil, and adding lead and silver to obtain a sample, wherein the adding amount of the lead is 40-60 times of the estimated copper weight in the gold cyanide mud sample, and the adding amount of the silver is such that the weight ratio of gold to silver in the sample is 1: (2.5-15);
(3) Preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the sample, adding copper with the same weight ratio as the sample according to the estimated copper content in the step (1), and putting the copper into lead foil with the same amount as the step (2);
(4) Blowing oxygen-enriched ash of the sample and the standard sample in a high-temperature melting state to obtain gold and silver alloy grains respectively, hammering the gold and silver alloy grains into slices or preparing alloy rolls, and then carrying out gold separation treatment to obtain sample gold and standard sample gold;
the gold content in the gold cyanide sludge sample was calculated according to the formula:
or (b)
When the weight difference between the sample and the standard sample is not more than 20mg, the gold content in the gold cyanide mud sample is calculated according to the following formula:
the omega (Au) is the mass fraction of gold in the gold cyanide mud sample, and the unit is M 1 The weight of the sample gold coil in the step (4) is mg and M 2 The mass of the cyanide gold mud sample weighed in the step (2) is expressed in mg,mean value of increment after separating gold for standard sample, +.>Mean value of F, increment after F and standard sample are separatedThe calculation formula of (2) is as follows:
F＝M 4 ×D/M 3 increment after standard sample gold separation = M 3 -M 4 ×D；
Wherein M is 3 The standard sample in the step (4) is expressed as mg and M 4 The weight of the pure gold in the standard sample in the step (3) is mg, and D is the mass fraction of the pure gold in the standard sample.
The standard sample gold and the sample gold can be gold coils or gold sheets, the gold coils are manufactured when the weight ratio of gold to silver is about 1:2.5, and the gold coils can be hammered into slices when the silver content becomes high.
According to the application, 40-60 times of lead is added according to the copper content in the gold cyanide mud sample to prepare the sample, so that the problem of abnormal detection results caused by the fact that metal oxide cannot be normally absorbed by a cupel due to abnormal surface tension of a melt caused by overhigh copper content in the high-temperature ash blowing process of the sample can be solved. The added lead can enable the surface tension of the solution to be stable, oxide can be normally absorbed by a cupel, the influence of the oxide on gold content is eliminated, and the influence factor in the detection process can be effectively eliminated by correcting a standard sample.
The silver was added so that the weight ratio of gold to silver in the sample was 1: (2.5-15), alloy sheets suitable for separating gold can be obtained in a beating and knocking mode, samples are not required to be rolled, the gold separation can be ensured to achieve a satisfactory effect in a mode of obtaining alloy sheets with uniform thickness through rolling, and the rolling effect of the alloy sheets in a ratio of 1:2.5 is better than that of beating into sheets. In the application, if the weight ratio of gold to silver exceeds 1:15, the gold separation speed is too high due to the too high silver content in the gold separation process, so that the probability of gold sheet breakage is increased, and damaged gold sheets are easy to lose in the subsequent operation, thereby leading to lower detection results. Therefore, the weight ratio of gold to silver is 1:
(2.5-15) the thickness of the alloy sheet is not so strict, and breakage is not easily caused during separating gold.
Optionally, in step (2), the lead is added in an amount of 50 times the estimated copper weight in the gold cyanide sludge sample.
Optionally, the weight ratio of the gold cyanide mud to the lead foil is 0.5-1:10-13.
Preferably, in the step (2), the weight ratio of the gold cyanide sludge to the lead foil is 0.5:13.
optionally, in the step (4), when the nickel content is 0.5%, the oxygen-enriched ash blowing treatment temperature is 1000 ℃, and when the nickel content is increased by 1%, the oxygen-enriched ash blowing treatment temperature is increased by 15-20 ℃ and the treatment time is 30-60min. The upper limit of the temperature of the oxygen-enriched ash blowing is 1150 ℃.
The temperature of the oxygen-enriched ash blowing is determined according to the nickel content, and when the nickel content is increased, the temperature of the oxygen-enriched ash blowing is increased, because nickel is not easy to oxidize, nitric acid is basically insoluble in nickel, and nickel exists in the finally obtained gold coil unless the nickel is not completely removed, so that the detection result of gold is higher.
Optionally, in the step (4), the gold and silver alloy particles are crushed into thin slices and are respectively put into a colorimetric tube, and gold separation treatment is sequentially carried out in a first nitric acid solution and a second nitric acid solution.
Optionally, the thickness of the sheet is 0.05-0.3mm, when the weight ratio of gold to silver is 1:2.5, the thickness of the sheet is 0.05-0.1mm, when the weight ratio of gold to silver is 1:2.5-5, the thickness of the sheet is 0.1-0.2mm, and when the weight ratio of gold to silver is higher than 1:5, the thickness of the sheet is 0.2-0.3mm.
The concentration of the first nitric acid solution is 1.6-1.9mol/L, the treatment temperature is 90-95 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 4.8-7.5mol/L, the treatment temperature is 90-95 ℃, and the treatment time is 30min.
The thickness of above-mentioned flake is convenient for improve the gold separation speed, and then practices thrift detection time, and first nitric acid solution's concentration is lower, can guarantee the integrality of flake, if the flake is broken then probably causes partial gold content unable to be counted for testing result is lower, and second nitric acid solution's concentration becomes higher, can realize quick gold separation to improve the purity of gold volume after the gold separation, thereby guarantee testing result's accuracy and precision.
Optionally, in the step (1), a noble metal instrument is adopted to predict the content of gold, silver and copper in the cyanide gold mud sample.
Optionally, in the step (1), weighing two gold cyanide mud samples with the weight of 500mg, directly wrapping one sample with more than 10g of lead to obtain a sample A, supplementing the silver amount with the weight of 5 times of gold according to a predicted value, wrapping the other sample with more than 10g of lead to obtain a sample B, respectively blowing the sample A and the sample B through high-temperature ash to obtain corresponding gold-silver composite particles, separating gold-silver composite particles of the sample B by nitric acid, and estimating the gold content and the silver content in the gold cyanide mud sample according to the weight of the gold-silver composite particles of the sample A and the weight of gold sheets obtained after separating gold from the sample B;
weighing 0.1g of gold cyanide mud sample, adding 10ml of nitric acid into a 200ml beaker to dissolve the sample, fixing the volume of pure water in a 100 ml colorimetric tube, measuring the copper concentration in the gold cyanide mud sample at the wavelength of 324.7nm on an atomic absorption spectrometer, and predicting the copper content in the gold cyanide mud sample.
The predicted value is predicted according to the numerical reference provided by a gold cyanide mud production workshop, the gold cyanide mud is a production flow product, and the gold and silver content in the gold cyanide mud can be judged according to the production condition, so that related information can be obtained from the production workshop, and the gold and silver content is relatively stable and has little change on the premise that the process and the raw materials are not changed greatly.
Optionally, the high-temperature ash blowing temperature is 900-1000 ℃ and the treatment time is 30-60min.
In actual production, if the sample contains copper and is added with more lead, the ash blowing time is properly prolonged, and the prolonged time is related to the added lead, and the time is prolonged by 5min after adding 10g of lead.
Preferably, the high-temperature ash blowing temperature is 950 ℃, and the treatment time is 40min.
The beneficial effects of the application include, but are not limited to:
1. according to the quantitative detection method provided by the application, the ash blowing process of the sample and the standard sample is finished in a constant-temperature and oxygen-enriched state, the added lead can ensure that the surface tension of molten liquid is normal in the ash blowing process, oxide can be normally absorbed by a cupel, and the gold content in the cyanide gold mud can be rapidly, accurately and quantitatively detected.
2. According to the quantitative detection method provided by the application, the same oxygen-enriched ash blowing and gold separation treatment are adopted for the sample and the standard sample, and the gold content is corrected by the incremental average value after gold separation of the standard sample, so that the accuracy and the precision of the detection method can be further improved, and the quantitative detection of the gold content in the gold cyanide mud is realized.
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 model of the atomic absorption spectrometer used in the application is ICE3300, and the manufacturer is Sieimer's femil;
the model of the noble metal analyzer is EDS7700T, and the manufacturer is the reputation.
The gold cyanide sludge used in the following examples and comparative examples was tested for a predicted gold content of 10-20% gold cyanide sludge. The method in the following examples and comparative examples was carried out on the direct cyanidation process, the roasting cyanidation process, and the resultant cyanidation gold mud samples (designated as sample No. 1 and sample No. 2, respectively).
Example 1
The embodiment relates to a method for quantitatively detecting gold content in gold cyanide mud, which comprises the following steps:
(1) A noble metal instrument is adopted to estimate the contents of gold, silver, copper and nickel in the gold cyanide mud sample;
(2) Preparing a sample: weighing a gold cyanide mud sample, and putting the gold cyanide mud sample into a lead foil, wherein the weight ratio of the gold cyanide mud to the lead foil is 0.5:13, adding lead and silver to obtain a sample, wherein the adding amount of the lead is 50 times of the estimated weight of copper in the gold cyanide mud sample, and the adding amount of the silver is such that the weight ratio of the gold to the silver in the sample is 1:8, 8;
(3) Preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the detection sample, adding copper with the same weight as the sample according to the estimated copper content in the step (1), and putting the copper into lead foil with the same amount as the step (2);
(4) Blowing the sample and the standard sample with oxygen-enriched ash in a high-temperature molten state to obtain gold-silver alloy particles respectively, smashing the gold-silver alloy particles into thin slices with the thickness of 0.05mm, respectively placing the thin slices into a colorimetric tube, and sequentially carrying out gold separation treatment in a first nitric acid solution and a second nitric acid solution to obtain a sample gold coil and a standard sample gold coil, wherein the concentration of the first nitric acid solution is 1.8mol/L, the treatment temperature is 90 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 7.0mol/L, the treatment temperature is 90 ℃, and the treatment time is 30min.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of example 1, and the gold content in the gold cyanide mud is calculated by two calculation formulas, wherein the result is shown in Table 1, and 1# -8# is a parallel experiment.
Table 1 example 1
Example 2
The embodiment relates to a method for quantitatively detecting gold content in gold cyanide mud, which comprises the following steps:
(1) A noble metal instrument is adopted to estimate the contents of gold, silver, copper and nickel in the gold cyanide mud sample;
(2) Preparing a sample: weighing a gold cyanide mud sample, and putting the gold cyanide mud sample into a lead foil, wherein the weight ratio of the gold cyanide mud to the lead foil is 0.5: adding lead and silver to obtain a sample, wherein the adding amount of the lead is 40 times of the estimated weight of copper in the gold cyanide mud sample, and the adding amount of the silver is such that the weight ratio of the gold to the silver in the sample is 1:10;
(3) Preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the detection sample, adding copper with the same weight as the sample according to the estimated copper content in the step (1), and putting the copper into lead foil with the same amount as the step (2);
(4) Blowing the sample and the standard sample with oxygen-enriched ash in a high-temperature molten state to obtain gold-silver alloy particles respectively, smashing the gold-silver alloy particles into thin slices with the thickness of 0.05mm, respectively placing the thin slices into a colorimetric tube, and sequentially carrying out gold separation treatment in a first nitric acid solution and a second nitric acid solution to obtain a sample gold coil and a standard sample gold coil, wherein the concentration of the first nitric acid solution is 1.6mol/L, the treatment temperature is 95 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 4.8mol/L, the treatment temperature is 95 ℃, and the treatment time is 30min.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are respectively detected by the method of example 2, and the gold content in the gold cyanide mud is respectively calculated by adopting two calculation formulas, the result is shown in Table 2, wherein 1# -8# is a parallel experiment.
Table 2 example 2
Example 3
The embodiment relates to a method for quantitatively detecting gold content in gold cyanide mud, which comprises the following steps:
(1) Weighing two gold cyanide mud samples with the weight of 500mg, directly wrapping one sample with more than 10g of lead to obtain a sample A, supplementing silver with the weight of 5 times of gold according to a predicted value, wrapping the other sample with more than 10g of lead to obtain a sample B, respectively carrying out ash blowing on the sample A and the sample B at the high temperature of 950 ℃ for 40min, separating gold by nitric acid, and predicting the gold and silver content in the gold cyanide mud sample;
weighing 0.1g of gold cyanide mud sample, adding 10ml of nitric acid into a 200ml beaker to dissolve the sample, fixing the volume of pure water in a 100 ml colorimetric tube, measuring the copper concentration and the nickel concentration in the gold cyanide mud sample by an atomic absorption spectrometer, and predicting the copper content and the nickel content in the gold cyanide mud sample;
(2) Preparing a sample: weighing a gold cyanide mud sample, and putting the gold cyanide mud sample into a lead foil, wherein the weight ratio of the gold cyanide mud to the lead foil is 1:13, adding lead and silver to obtain a sample, wherein the adding amount of the lead is 60 times of the estimated copper weight in the gold cyanide mud sample, and the adding amount of the silver is such that the weight ratio of the gold to the silver in the sample is 1:5, a step of;
(3) Preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the detection sample, adding copper with the same proportion as the sample according to the estimated copper content in the step (1), and putting the copper into lead foil with the same amount as the step (2);
(4) Blowing the sample and the standard sample with oxygen-enriched ash in a high-temperature molten state to obtain gold-silver alloy particles respectively, smashing the gold-silver alloy particles into thin slices with the thickness of 0.1mm, respectively placing the thin slices into a colorimetric tube, and sequentially carrying out gold separation treatment in a first nitric acid solution and a second nitric acid solution to obtain a sample gold coil and a standard sample gold coil, wherein the concentration of the first nitric acid solution is 1.9mol/L, the treatment temperature is 90 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 7.5mol/L, the treatment temperature is 90 ℃, and the treatment time is 30min.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of example 3, and the gold content in the gold cyanide mud is calculated by two calculation formulas, the result is shown in Table 3, wherein 1# -8# is a parallel experiment.
TABLE 3 example 3
Example 4
This embodiment differs from embodiment 1 in that: in the step (2), the weight ratio of the gold cyanide mud to the lead foil is 0.5:5, the rest of procedure is the same as in example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of example 4, and the gold content in the gold cyanide mud is calculated by two calculation formulas, the result is shown in Table 4, wherein 1# -8# is a parallel experiment.
Table 4 example 4
Example 5
This embodiment differs from embodiment 1 in that: in the step (4), the thickness of the sheet was 0.5mm, and the rest of the procedure was the same as in example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of example 5, and the gold content in the gold cyanide mud is calculated by two calculation formulas, the result is shown in Table 5, wherein 1# -8# is a parallel experiment.
TABLE 5 example 5
Example 6
This embodiment differs from embodiment 1 in that: in the step (4), the concentration of the first nitric acid solution is 7.0mol/L, the treatment temperature is 90 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 1.8mol/L, the treatment temperature is 90 ℃, the treatment time is 30min, and the rest steps are the same as those in the example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of example 6, and the gold content in the gold cyanide mud is calculated by two calculation formulas, the result is shown in Table 6, wherein 1# -8# is a parallel experiment. In this embodiment, the concentration of the first nitric acid solution is greater than that of the second nitric acid solution, so that the gold flakes of sample No. 1 and sample No. 2 are broken in one gold separation process, but the result of weighing sample No. 1 is found to be obviously lower than that of sample No. 3 and sample No. 6, and sample No. 2 is caused by loss in the gold flake transfer process, so that the data are discarded.
TABLE 6 example 6
Comparative example 1
The difference between this comparative example and example 1 is that: in the step (2), the addition amount of lead is 10 times of the estimated copper weight in the gold cyanide mud sample, and the rest of the steps are the same as in the example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of comparative example 1, and the gold content in the gold cyanide mud is calculated by two calculation formulas, wherein the result is shown in Table 7, and 1# -8# is a parallel experiment.
Table 7 comparative example 1
Comparative example 2
The difference between this comparative example and example 1 is that: in the step (2), the addition amount of lead is 70 times of the estimated copper weight in the gold cyanide mud sample, and the rest of the steps are the same as in the example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 and the sample No. 3 are detected by the method of comparative example 2, and the gold content in the gold cyanide mud is calculated by two calculation formulas, the result is shown in Table 8, wherein 1# -8# is a parallel experiment.
Table 8 comparative example 2
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Comparative example 3
The difference between this comparative example and example 1 is that: in the step (2), the weight ratio of gold to silver in the sample is 1:20, the rest of procedure is the same as in example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of comparative example 3, and the gold content in the gold cyanide mud is calculated by two calculation formulas, wherein the result is shown in Table 9, and 1# -8# is a parallel experiment. Since the weight ratio of gold to silver was increased in this example, the parallel experiments # 2, # 3 and # 7 for sample No. 1 and the parallel experiments # 2, # 4, # 5 and # 7 for sample No. 2 all showed that the cash piece was broken, and the deviation of the test results from the test data for sample No. 2 was large, so that the data was discarded.
Table 9 comparative example 3
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Comparative example 4
The difference between this comparative example and example 1 is that: the same proportion of copper as that of the sample was not added in step (3), and the rest of the procedure was the same as in example 1.
The weight difference between the sample and the standard sample is not more than 20mg, the sample No. 1 and the sample No. 2 are detected by the method of comparative example 4, and the gold content in the gold cyanide mud is calculated by two calculation formulas, wherein the result is shown in Table 10, and 1# -8# is a parallel experiment.
Table 10 comparative example 4
Comparative example 5
The difference between this comparative example and example 1 is that: step (3) was not performed, and the content of the gold cyanide mud sample was calculated as follows, as in example 1:
ω(Au)＝[M 1 /M 2 ]×100。
sample No. 1 and sample No. 2 were tested by the method of comparative example 5, and the results are shown in table 11, wherein 1# -8# is a parallel experiment.
Table 11 comparative example 5
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Comparative example 6
The method for detecting the gold by adopting the fire test method of alloy comprises weighing the sample according to the gold content of 300mg in the sample, adopting the ratio of gold to silver of 1:2.5, adding copper and nickel which are consistent with the weight of the sample into a correction standard sample, adding lead with the copper content of 50 times into the sample and the standard sample, and detecting the sample No. 1-No. 2 to obtain the gold content, wherein the result is shown in Table 12, and 1# 8 is a parallel experiment.
Table 12 comparative example 6
According to the results, the detection method can realize rapid quantitative detection of gold cyanide mud, and meets the requirements of repeatability limit and reproducibility limit of the gold content range of the sample in the related national and industry standard detection method. Compared with a fire gold test method adopting GB/T7739.1-2019 gold concentrate, the detection method provided by the application has the advantages of lower detection cost, shorter detection time and simpler and more convenient operation.
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. The method for quantitatively detecting the gold content in the gold cyanide mud is characterized by comprising the following steps of:
(1) Estimating the content of gold, silver, copper and nickel in the cyanide gold mud sample;
(2) Preparing a sample: weighing a gold cyanide mud sample, putting the gold cyanide mud sample into a lead foil, and adding lead and silver to obtain a sample, wherein the adding amount of the lead is 40-60 times of the estimated copper weight in the gold cyanide mud sample, and the adding amount of the silver is such that the weight ratio of gold to silver in the sample is 1: (2.5-15);
(3) Preparing a standard sample: mixing pure gold and pure silver with the same weight ratio as the sample, adding copper with the same weight ratio as the sample according to the estimated copper content in the step (1), and putting the copper into lead foil with the same amount as the step (2);
(4) Blowing oxygen-enriched ash of the sample and the standard sample in a high-temperature melting state to obtain gold and silver alloy grains respectively, hammering the gold and silver alloy grains into slices or preparing alloy rolls, and then carrying out gold separation treatment to obtain sample gold and standard sample gold;
the gold content in the gold cyanide sludge sample was calculated according to the formula:
or (b)
When the weight difference between the sample and the standard sample is not more than 20mg, the gold content in the gold cyanide mud sample is calculated according to the following formula:
the omega (Au) is gold cyanideThe mass fraction of gold in the mud sample is expressed as M 1 The weight of the gold sample in the step (4) is mg, M 2 The mass of the cyanide gold mud sample weighed in the step (2) is expressed in mg,mean value of increment after separating gold for standard sample, +.>The average value of F is calculated as follows:
F＝M 4 ×D/M 3 increment after standard sample gold separation = M 3 -M 4 ×D；
Wherein M is 3 The standard sample in the step (4) is expressed as mg and M 4 The weight of the pure gold in the standard sample in the step (3) is mg, and D is the mass fraction of the pure gold in the standard sample.
2. The method of claim 1, wherein in step (2) the lead is added in an amount of 50 times the estimated copper weight in the gold cyanide sludge sample.
3. The method according to claim 1, wherein in step (2), the weight ratio of the gold cyanide sludge to the lead foil is 0.5-1:10-13.
4. A method according to claim 3, wherein in step (2), the weight ratio of the gold cyanide sludge to the lead foil is 0.5:13.
5. the method according to claim 1, wherein in the step (4), when the nickel content is 0.5%, the oxygen-enriched ash blowing treatment temperature is 1000 ℃, and the nickel content is increased by 1%, the oxygen-enriched ash blowing treatment temperature is increased by 15-20 ℃, the upper limit of the oxygen-enriched ash blowing treatment temperature is 1150 ℃, and the treatment time is 30-60min.
6. The method according to claim 1, wherein in the step (4), the gold and silver alloy particles are crushed into thin slices and respectively put into a cuvette, and gold separation treatment is sequentially performed in a first nitric acid solution and a second nitric acid solution.
7. The method of claim 6, wherein the lamina has a thickness of 0.2-0.3mm;
the concentration of the first nitric acid solution is 1.6-1.9mol/L, the treatment temperature is 90-95 ℃, the treatment time is 30min, the concentration of the second nitric acid solution is 4.8-7.5mol/L, the treatment temperature is 90-95 ℃, and the treatment time is 30min.
8. The method of claim 1, wherein in step (1), the precious metal meter is used to estimate the gold, silver, and copper content of the gold cyanide sludge sample.
9. The method according to claim 1, wherein in the step (1), two gold cyanide mud samples with the weight of 500mg are weighed, one sample is directly wrapped with more than 10g of lead to obtain a sample A, the other sample is added with silver with the weight of 5 times of gold according to a predicted value, more than 10g of lead is wrapped to obtain a sample B, the sample A and the sample B are respectively subjected to high-temperature ash blowing to obtain corresponding gold-silver alloy particles, gold-silver alloy particles of the sample B are subjected to gold separation by nitric acid, and the gold and silver content in the gold cyanide mud samples is estimated according to the weight of the gold-silver alloy particles of the sample A and the weight of gold pieces obtained after gold separation of the sample B;
weighing 0.1g of gold cyanide mud sample, adding 10ml of nitric acid into a 200ml beaker to dissolve the sample, fixing the volume of pure water in a 100 ml colorimetric tube, measuring the copper concentration in the gold cyanide mud sample at the wavelength of 324.7nm on an atomic absorption spectrometer, and predicting the copper content in the gold cyanide mud sample.
10. The method according to claim 1, wherein the high temperature ash blowing temperature is 900-1000 ℃ and the treatment time is 30-60min.
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