CN109085033A - A kind of complicated difficult soluble noble metal standard sample preparation method and its content test method - Google Patents
A kind of complicated difficult soluble noble metal standard sample preparation method and its content test method Download PDFInfo
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- CN109085033A CN109085033A CN201810951440.3A CN201810951440A CN109085033A CN 109085033 A CN109085033 A CN 109085033A CN 201810951440 A CN201810951440 A CN 201810951440A CN 109085033 A CN109085033 A CN 109085033A
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- sample
- noble metal
- standard sample
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- soluble noble
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- 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
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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
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Abstract
The invention belongs to noble metal sample pretreating technical fields, and in particular to a kind of complicated difficult soluble noble metal standard sample preparation method and its content test method.This kind of complicated difficult soluble noble metal standard sample preparation method in sample making course by using adding a certain proportion of fluxing agent (lithium tetraborate and lithium metaborate mixture) slag making under high temperature fused state, make metal and nonmetallic is all mixed in slag, by being crushed to slag, being ground up, sieved to obtain standard sample, solve traditional handicraft metal and the nonmetallic complicated sample preparation process separated, simultaneously using bullion content in Fire Assaying test technology testing standard sample, accomplish quick, accurate test valuable metal content.
Description
Technical field
The invention belongs to noble metal sample pretreating technical fields, and in particular to a kind of complicated difficult soluble noble metal standard sample system
Preparation Method and its content test method.
Background technique
Noble metal has 8 chemical elements: Au Ag Pt Pd, rhodium, iridium, ruthenium and osmium, since the industrial application of osmium is considerably less,
Be related in the market the secondary resource waste of osmium almost without, research in relation to osmium and application documents and materials are considerably less, actually I
The noble metal that refers to be 7 chemical elements in addition to osmium.
Precious metal palladium and silver can be dissolved by nitric acid, and gold, platinum and palladium can be by aqua regia dissolution, the chemolysis of gold, silver, platinum and palladium
Property more other precious metal element rhodiums, iridium and ruthenium it is relatively easy, gold, silver, the pre-treatment of platinum and palladium analysis sample and its separating-purifying
Relatively easily, due to rhodium, iridium and ruthenium chemical property very inertia, rhodium, the pretreatment technology of iridium and ruthenium analysis sample and its separation
It purifies extremely complex.
When preparing quantitative analysis noble metal secondary resource material, pre-treatment will be carried out to analysis sample, make to analyze sample
In noble metal be completely converted into soluble state, then using chemical dissolution method make sample all dissolution enter solution, finally
Analyzed in assay laboratory using instrument: electric induction lotus root closes emission spectrometer ICP or Atomic Absorption Spectrometer AA etc., or chemistry point
The concentration for analysing noble metal in Accurate Determining solution calculates the content of noble metal in sample according to the data of pretreatment process.It is complicated
The analysis of Precious Metals Sample Pretreatment Technique main method of indissoluble has fire assaying and high-temperature melting method.
Before the Noble Metal Rhodium, iridium and the ruthenium analysis sample that disclose a kind of complicated indissoluble such as patent No. CN201710881498.0
Processing method.Noble Metal Rhodium, iridium and the ruthenium of complicated indissoluble analyze sample-pretreating method, successively carry out as follows: A, fixed
Property analysis；B, it roasts；C, it restores；D, it grinds；E, high-temperature fusion；F, it dissolves.Operation of the present invention is simple, and analytical technology personnel are easy
Grasp whole process；Sample pre-treatments solution is Clear & Transparent, and sample is completely dissolved；Analysis of Precious Metals result precision is high, but institute
The sample-pretreating method sample preparation process stated is complicated, and is not directed to the sample making course of complex sample.
Summary of the invention
Uneven in order to solve above-mentioned sample, the problems such as sample complexity is not easy to handle, and sample preparation process is complicated, the present invention provides
A kind of complicated difficult soluble noble metal standard sample preparation method and its content test method.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of complicated difficult soluble noble metal standard sample system
Preparation Method, comprising the following steps:
S1: weighing analysis sample m1 to be measured, crushes, and is placed in clean glassware；
S2: weighing and be pre-mixed uniform mixed flux m2 in the glassware in step S1, is sufficiently mixed uniformly；
S3: the sample being uniformly mixed in S2 being transferred in the crucible of quality m0, heats 30-50min；
S4: crucible in step S3 is taken out, and is cooled to room temperature to obtain slag, is weighed m3；
S5: by slag break process in step S4, and it is multiple using quartering division, until retaining sample m4；
S6: sample grinding will be retained in step S5 and sieve to obtain 100-150 mesh standard sample.
Further, analysis sample to be measured includes waste and old pcb board, FPC plate, chip in step S1.
Further, the analysis sample granularity≤3mm to be measured crushed in step S1.
Further, mixed flux includes lithium tetraborate and lithium metaborate in step S2.
Further, the mass ratio of lithium tetraborate and lithium metaborate is 1:1~3:1.
Further, the mass ratio m1:m2=1:4~1:8 to be measured for analyzing sample and mixed flux in step S1 and S2.
Further, crucible includes oxidation zirconium crucible in step S4.
Further, crucible is placed in Muffle furnace and heats in step S4, and heating temperature is 700-1000 DEG C.
Further, the mass ratio m1:m4=to be measured for analyzing sample and quartering division reservation sample in step S1 and S5
1:1.5~1:3.
Further, the mesh number of step S6 Plays sample is 120 mesh.
A kind of complicated difficult soluble noble metal sample content test method uses above-mentioned any one complicated difficult soluble noble metal mark
The bullion content ρ of standard sample prepared by quasi- preparation method of sample；Bullion content in analysis sample to be tested are as follows: ω=
(m3-m0) × ρ/m1, m3 is slag and quality in formula, and m0 is quality, and ρ is bullion content in standard sample, m1
For analysis sample mass to be measured.
Further, the bullion content ρ application Fire Assaying test technology measuring and calculating of standard sample.
The present invention provides a kind of complicated difficult soluble noble metal standard sample preparation method and its content test method, by using
A certain proportion of fluxing agent (lithium tetraborate and lithium metaborate mixture) is added in sample making course to make under high temperature fused state
Slag, make metal and it is nonmetallic be all mixed in slag, by being crushed to slag, being ground up, sieved to obtain standard sample, solve biography
It unites process metal and the nonmetallic complicated sample preparation process separated, while your gold in Fire Assaying test technology testing standard sample is applied
Belong to content, accomplishes quick, accurate test valuable metal content.
Detailed description of the invention
Fig. 1 is the flow chart of one complicated difficult soluble noble metal standard sample preparation method of embodiment；
Fig. 2 is the flow chart of two complicated difficult soluble noble metal standard sample preparation method of embodiment；
Fig. 3 is the flow chart of three complicated difficult soluble noble metal standard sample preparation method of embodiment.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, is clearly and completely retouched to the technical solution in the present invention
It states, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.
It is illustrated so that analysis sample to be measured is waste and old pcb board as an example below.
Embodiment one
As shown in Figure 1, a kind of complicated difficult soluble noble metal standard sample preparation method, comprising the following steps:
S1: weighing 100g and crush to obtain granularity≤3mm waste and old pcb board of analysis sample to be measured, is placed in clean wide-mouth bottle
In；
S2: weighing 500g and be pre-mixed uniform mixed flux in the wide-mouth bottle in step S1, is sufficiently mixed uniformly,
The mass ratio of the mixed flux lithium tetraborate and lithium metaborate is 1:1；
S3: the sample being uniformly mixed in S2 is transferred in the oxidation zirconium crucible of quality 200g, and is placed in Muffle furnace
850 DEG C are heated to, 40min is kept；
S4: crucible in step S3 is taken out, and is cooled to room temperature to obtain slag, is weighed 850g；
S5: using simple crushing tool for slag in step S4, if hammer or medicinal crusher carry out simple crushing processing,
And it is multiple using quartering division, until retaining sample 200g；
S6: by step S5 retain sample grinding sieve 120 mesh standard sample.
A kind of complicated difficult soluble noble metal sample content test method, the mark of above-mentioned preparation is tested using Fire Assaying test technology
Quasi- sample bullion content ρ, bullion content is tested according to professional standard YS/T745.2 Fire Assaying in sample, Au test result
For 50g/t.
According to formula: ω=(m3-m0) × ρ/m1, m3 is slag and quality in formula, and m0 is quality, and ρ is mark
Bullion content in quasi- sample, m1 are analysis sample mass to be measured, calculate bullion content in analysis sample to be tested are as follows: ω=
(850-200) × 50/100=325g.
Embodiment two
As shown in Fig. 2, a kind of complicated difficult soluble noble metal standard sample preparation method, comprising the following steps:
S1: weighing 100g and crush to obtain granularity≤3mm waste and old pcb board of analysis sample to be measured, is placed in clean wide-mouth bottle
In；
S2: weighing 500g and be pre-mixed uniform mixed flux in the wide-mouth bottle in step S1, is sufficiently mixed uniformly,
The mass ratio of the mixed flux lithium tetraborate and lithium metaborate is 2:1；
S3: the sample being uniformly mixed in S2 is transferred in the oxidation zirconium crucible of quality 200g, and is placed in Muffle furnace
750 DEG C are heated to, 40min is kept；
S4: crucible in step S3 is taken out, and is cooled to room temperature to obtain slag, is weighed 850g；
S5: using simple crushing tool for slag in step S4, if hammer or medicinal crusher carry out simple crushing processing,
And it is multiple using quartering division, until retaining sample 200g；
S6: sample grinding will be retained in step S5 and sieve to obtain 120 mesh standard samples.
A kind of complicated difficult soluble noble metal sample content test method, the mark of above-mentioned preparation is tested using Fire Assaying test technology
Quasi- sample bullion content ρ, bullion content is tested according to professional standard YS/T745.2 Fire Assaying in sample, Au test result
For 50g/t.
According to formula: ω=(m3-m0) × ρ/m1, m3 is slag and quality in formula, and m0 is quality, and ρ is mark
Bullion content in quasi- sample, m1 are analysis sample mass to be measured, calculate bullion content in analysis sample to be tested are as follows: ω=
(850-200) × 50/100=325g.
Embodiment three
As shown in figure 3, a kind of complicated difficult soluble noble metal standard sample preparation method, comprising the following steps:
S1: weighing 100g and crush to obtain granularity≤3mm waste and old pcb board of analysis sample to be measured, is placed in clean wide-mouth bottle
In；
S2: weighing 500g and be pre-mixed uniform mixed flux in the wide-mouth bottle in step S1, is sufficiently mixed uniformly,
The mass ratio of the mixed flux lithium tetraborate and lithium metaborate is 3:1；
S3: the sample being uniformly mixed in S2 is transferred in the oxidation zirconium crucible of quality 200g, and is placed in Muffle furnace
700 DEG C are heated to, 40min is kept；
S4: crucible in step S3 is taken out, and is cooled to room temperature to obtain slag, is weighed 850g；
S5: using simple crushing tool for slag in step S4, if hammer or medicinal crusher carry out simple crushing processing,
And it is multiple using quartering division, until retaining sample 200g；
S6: by step S5 retain sample grinding sieve 120 mesh standard sample.
A kind of complicated difficult soluble noble metal sample content test method, the mark of above-mentioned preparation is tested using Fire Assaying test technology
Quasi- sample bullion content ρ, bullion content is tested according to professional standard YS/T745.2 Fire Assaying in sample, Au test result
For 50g/t.
According to formula: ω=(m3-m0) × ρ/m1, m3 is slag and quality in formula, and m0 is quality, and ρ is mark
Bullion content in quasi- sample, m1 are analysis sample mass to be measured, calculate bullion content in analysis sample to be tested are as follows: ω=
(850-200) × 50/100=325g.
Therefore, the present invention in sample making course by using adding a certain proportion of fluxing agent (lithium tetraborate and metaboric acid
Lithium mixture) slag making under high temperature fused state, make metal and it is nonmetallic be all mixed in slag, by being crushed, being ground to slag
Mill, sieving obtain standard sample, solve traditional handicraft metal and the nonmetallic complicated sample preparation process separated, while application fire examination
Bullion content in golden test technology testing standard sample accomplishes quick, accurate test valuable metal content.
It above are only preferred embodiment of the invention, but the design concept of the present invention is not limited to this, all benefits
It is made a non-material change to the present invention, should all be belonged to behavior that violates the scope of protection of the present invention with this design.
Claims (12)
1. a kind of complicated difficult soluble noble metal standard sample preparation method, it is characterised in that: the following steps are included:
S1: weighing analysis sample m1 to be measured, crushes, and is placed in clean glassware；
S2: weighing and be pre-mixed uniform mixed flux m2 in the glassware in step S1, is sufficiently mixed uniformly；
S3: the sample being uniformly mixed in S2 being transferred in the crucible of quality m0, heats 30-50min；
S4: crucible in step S3 is taken out, and is cooled to room temperature to obtain slag, is weighed m3；
S5: by slag break process in step S4, and it is multiple using quartering division, until retaining sample m4；
S6: will in step S5 retain sample grinding sieve mesh number be 100-150 mesh, obtain standard sample.
2. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S1
In analysis sample to be measured include waste and old pcb board, FPC plate, chip.
3. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S1
It is middle to crush obtained analysis sample granularity≤3mm to be measured.
4. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S2
Middle mixed flux includes lithium tetraborate and lithium metaborate.
5. complicated difficult soluble noble metal standard sample preparation method according to claim 4, it is characterised in that: the tetraboric acid
The mass ratio of lithium and lithium metaborate is 1:1~3:1.
6. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S1
With mass ratio m1:m2=1:4~1:8 of analysis sample and mixed flux to be measured in S2.
7. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S4
Middle crucible includes oxidation zirconium crucible.
8. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S4
Middle crucible, which is placed in Muffle furnace, to be heated, and heating temperature is 700-1000 DEG C.
9. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step S1
Retain mass ratio m1:m4=1:1.5~1:3 of sample with analysis sample to be measured in S5 and quartering division.
10. complicated difficult soluble noble metal standard sample preparation method according to claim 1, it is characterised in that: the step
The mesh number of S6 Plays sample is 120 mesh.
11. a kind of complicated difficult soluble noble metal sample content test method, it is characterised in that: appoint using described in claim 1-10
Anticipate the bullion content ρ of standard sample prepared by a complicated difficult soluble noble metal standard sample preparation method；Analysis to be tested
Bullion content in sample are as follows: ω=(m3-m0) × ρ/m1, m3 is slag and quality in formula, and m0 is quality, and ρ is
Bullion content in standard sample, m1 are analysis sample mass to be measured.
12. complicated difficult soluble noble metal sample content test method according to claim 11, it is characterised in that: the standard
The bullion content ρ application Fire Assaying test technology of sample is calculated.
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| CN113654942A (en) * | 2021-09-06 | 2021-11-16 | 珠海格力绿色再生资源有限公司 | Method for testing content of noble metal in bridge chip circuit board and sample preparation method |
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