CN1696638A - Standard pattern of emission spectrum of pure silver, and preparation method - Google Patents
Standard pattern of emission spectrum of pure silver, and preparation method Download PDFInfo
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- CN1696638A CN1696638A CN200510020915.XA CN200510020915A CN1696638A CN 1696638 A CN1696638 A CN 1696638A CN 200510020915 A CN200510020915 A CN 200510020915A CN 1696638 A CN1696638 A CN 1696638A
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Abstract
A standard sample of pure Ag emitted spectrum is compose of 0.00045 - 0.018 Au, 0.00010 - 0.041 Cu, 0.00055 - 0.011 Fe, 0.00012 -0.042 Pb, 0.00045 - 0.0090 Sb, 0.00040 - 0.0165 Bi, 0.0005 - 0.0082 Pd, 0.0003 - 0.0081 Se, 0.0004 - 0.0081 Te, 0.00045 - 0.0080 Zn and Ag base as allowance by wt %. The said Ag base is pure Ag containing 99.995 % Ag content and the other metals are pure metals containing 99.99 % metal content.
Description
Technical field:
The present invention is relevant with standard model, and is special relevant with standard pattern of emission spectrum of pure silver and preparation method thereof.
Background technology:
According to domestic and international analytical technology state of development, the conventional analysis of row bulk article is the most effective a kind of means when using the emission spectrum method, and its split pole is a key problem of silver production field with the development of material standard sample.Fine silver spectral analysis standard model is that silver is smelted the indispensable standard matter of check analysis.Under the situation of China's bullion market relieving, silver smelting producer in all parts of the country is increasing, and except that the strong big smeltery of a part had direct-reading spectrometer, most of manufacturer all adopted spectrography that the composition of fine silver is carried out split pole.Because standard GB/T4135-2002 " silver " issued on September 17th, 2002, on April 1st, 2003 implemented.New national standard has been made requirement for the copper in the fine silver (Cu), bismuth (Bi), iron (Fe), plumbous (Pb), antimony (Sb), palladium (Pd), selenium (Se), eight kinds of elements of tellurium (Te), and wherein palladium, selenium, three kinds of elements of tellurium increase newly.Because the revision of national standard, original fine silver spectral analysis can not adapt to request of national standard with standard model.
Summary of the invention:
The objective of the invention is in order to overcome above deficiency, a kind of standard pattern of emission spectrum of pure silver that can adapt to national new standard requirement is provided.Another object of the present invention is for a kind of preparation method of standard pattern of emission spectrum of pure silver is provided.
The object of the present invention is achieved like this:
Standard pattern of emission spectrum of pure silver of the present invention, make by following raw material by weight percentage:
Gold 0.00045～0.018,
Copper 0.00010～0.041,
Iron 0.00055～0.011,
Lead 0.0012～0.042,
Antimony 0.00045～0.0090,
Bismuth 0.00040～0.0165,
Palladium 0.0005～0.0082,
Selenium 0.0003～0.0081,
Tellurium 0.0004～0.0081,
Zinc 0.00045～0.0080,
The silver matrix surplus.
Above-mentioned silver matrix is that silver content is at least 99.995% fine silver, and other metal is that tenor is at least 99.99% simple metal.
Make by following raw material by weight percentage in the above-mentioned sample:
Gold 0.00049,
Copper 0.00012,
Iron 0.00064,
Lead 0.0013,
Antimony 0.00049,
Bismuth 0.00042,
Palladium 0.00051,
Selenium 0.0004,
Tellurium 0.00045,
Zinc 0.00048,
The silver matrix surplus.
Make by following raw material by weight percentage in the above-mentioned sample:
Gold 0.0011,
Copper 0.0024,
Iron 0.0013,
Lead 0.0025,
Antimony 0.00098,
Bismuth 0.00099,
Palladium 0.001,
Selenium 0.00088,
Tellurium 0.0009,
Zinc 0.00098,
The silver matrix surplus.
Make by following raw material by weight percentage in the above-mentioned sample:
Gold 0.0020,
Copper 0.0049,
Iron 0.0026,
Lead 0.0051,
Antimony 0.0021,
Bismuth 0.0021,
Palladium 0.0021,
Selenium 0.0019,
Tellurium 0.00199,
Zinc 0.0021,
The silver matrix surplus.
Make by following raw material by weight percentage in the above-mentioned sample:
Gold 0.0039,
Copper 0.0106,
Iron 0.0049,
Lead 0.0104,
Antimony 0.0043,
Bismuth 0.0042,
Palladium 0.004,
Selenium 0.0039,
Tellurium 0.00387,
Zinc 0.0041,
The silver matrix surplus.
Make by following raw material by weight percentage in the above-mentioned sample:
Gold 0.0081,
Copper 0.0199,
Iron 0.0099,
Lead 0.0206,
Antimony 0.0082,
Bismuth 0.0081,
Palladium 0.0079,
Selenium 0.0077,
Tellurium 0.0079,
Zinc 0.0079,
The silver matrix surplus.
The preparation method of standard pattern of emission spectrum of pure silver of the present invention comprises the steps:
1), the selection of raw material: selecting silver content for use is that 99.995% fine silver is a silver matrix, and other metal selects for use tenor to be at least 99.9% simple metal;
2), batching: prepare burden in proportion;
3), founding: use medium-frequency induction furnace, after body of heater and the preheating of carbon crucible, add fine silver raw material and fusing earlier, then other raw material is added in the carbon crucible simultaneously, treat that fusing evenly and reach to take out rapidly behind 1100 ℃～1300 ℃ of the cast temperatures and adopt the combined type mold to cast promptly to make corresponding standard pattern of emission spectrum of pure silver, also can adopt other casting method.
Above-mentioned medium-frequency induction furnace adopts the 50KW medium-frequency induction furnace, and cast temperature is 1200 ℃.
Above-mentioned combined type mold comprises amalgamation successively and at least two moulds that connect by web member, above the mosaic between adjacent molds diversion groove is arranged, the plug hole that is communicated with diversion groove.
On the above-mentioned mold pilot hole is arranged.
Standard pattern of emission spectrum of pure silver of the present invention has added gold, copper, bismuth, iron, lead, ladder, palladium, selenium, tellurium, ten kinds of metals of zinc in silver matrix, compare with original standard model, has increased by 4 kinds of raw materials.Test by analysis, standard pattern of emission spectrum of pure silver of the present invention can adapt to the requirement of national new standard GB/TB135-2002 " silver ", is suitable for very much the analysis to fine silver composition in the silver-colored bulk article.The inventive method can be produced qualified standard pattern of emission spectrum of pure silver.
Description of drawings:
Fig. 1 is the goldstandard curve synoptic diagram.
Fig. 2 is a bismuth typical curve synoptic diagram.
Fig. 3 is a copper typical curve synoptic diagram.
Fig. 4 is an iron typical curve synoptic diagram.
Fig. 5 is a selenium typical curve synoptic diagram.
Fig. 6 is a tellurium typical curve synoptic diagram.
Fig. 7 is plumbous typical curve synoptic diagram.
Fig. 8 is a palladium typical curve synoptic diagram.
Fig. 9 is an antimony typical curve synoptic diagram.
Figure 10 is a zinc typical curve synoptic diagram.
Figure 11 is five assembly combined type casting die structure synoptic diagram.
Figure 12 is the vertical view of Figure 11.
Embodiment:
Standard pattern of emission spectrum of pure silver embodiment of the present invention sees Table 1.
Table 1:
What above silver matrix adopted is that silver content is at least 99.995% fine silver, and other tenor is at least 99.9% simple metal.
The preparation method of above-mentioned sample comprises the steps:
1): select materials: selecting silver content for use is that 99.995% fine silver is a silver matrix, and other metal selects for use content to be at least 99.9% simple metal;
2), batching: prepare burden in proportion;
3), founding: use the 50KW medium-frequency induction furnace, after body of heater and the preheating of carbon crucible, add fine silver raw material and fusing earlier, then other raw material is added in the carbon crucible simultaneously, wait to melt evenly and reach and take out that adopting casts as Figure 11, combined type mold shown in Figure 12 promptly makes corresponding standard pattern of emission spectrum of pure silver behind 1200 ℃ of the cast temperatures rapidly.
Requirement according to GB/T1500.5-1994 " chemical analysis standard model technology general rule ", adopt the on-board check range method to carry out the homogeneity inspection to sample, measure the content intensity data of 10 kinds of raw materials in the sample respectively, and calculate, the result shows that the distribution of 10 kinds of raw materials all is uniform.
Fig. 1～Figure 10 is the working curve of the standard model of according to standard sample value data formulation.As can be seen from Figure, the content distribution of 10 kinds of raw materials is reasonable, and working curve is linear good.
Figure 11, Figure 12 have provided five and have pieced together combined type casting die structure synoptic diagram.Referring to Figure 11, Figure 12, present embodiment combined type mold adopts the cast iron materials manufacturing, by five independently mould 1 be put together.This mold each side has two screws 2 that are used for fastening mould, and screw 3 screw threads are through in the screw each mould is linked into an integrated entity.In the middle of screw a pilot hole 4 is arranged respectively, keeper 5 is contained in the pilot hole.This design can guarantee that distortion does not appear in mould in casting cycle, guarantees that bar-shaped standard model meets the physical dimension requirement.Between the adjacent molds of mold top diversion groove 6 is arranged, be interconnected between diversion groove.100 tapping holes 7 are communicated with diversion groove.Can guarantee that the melt metal liquation utilizes self gravitation to flow into fast in the tapping hole, makes standard model have good homogeneous.100 of bar-shaped standard samples for spectrochemical analysis that can disposable casting conforms to quality requirements (Φ=6mm, H=110mm).Before mold uses, need roasting heat and fumigation on hot plate.
Fine silver matrix and each impurity element intermediate alloy of having weighed are added medium-frequency induction furnace, wait to melt the back and fully stir; The preheating on electric furnace earlier of combined type mold makes the evenly smoked last layer black Haze of mould inner mould wall with the acetylene flame then, tightens mold.The noble metal liquation is evenly poured in the mold along diversion groove, and attention casting liquid stream wants steady, can not stop, and allows the interior gas of mould fully discharge.After casting is finished, in mold, take out register pin, unclamp holding screw, therefrom separate sectional die, take out the bar-shaped silver-colored standard sample for spectrochemical analysis of having cast, after preliminary finishing, get final product.
The various embodiments described above are that foregoing of the present invention is further described, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (10)
1, standard pattern of emission spectrum of pure silver is characterized in that being made by following raw material by weight percentage:
Gold 0.00045～0.018,
Copper 0.00010～0.041,
Iron 0.00055～0.011,
Lead 0.0012～0.042,
Antimony 0.00045～0.0090,
Bismuth 0.00040～0.0165,
Palladium 0.0005～0.0082,
Selenium 0.0003～0.0081,
Tellurium 0.0004～0.0081,
Zinc 0.00045～0.0080,
The silver matrix surplus.
Above-mentioned silver matrix is that silver content is at least 99.995% fine silver, and other metal is that tenor is at least 99.99% simple metal.
2, the pure standard sampler of emitting spectroscopy of penetrating according to claim 1 is characterized in that being made by following raw material by weight percentage:
Gold 0.00049,
Copper 0.00012,
Iron 0.00064,
Lead 0.0013,
Antimony 0.00049,
Bismuth 0.00042,
Palladium 0.00051,
Selenium 0.0004,
Tellurium 0.00045,
Zinc 0.00048,
The silver matrix surplus.
3, standard pattern of emission spectrum of pure silver as claimed in claim 1 is characterized in that being made by following raw material by weight percentage:
Gold 0.0011,
Copper 0.0024,
Iron 0.0013,
Lead 0.0025,
Antimony 0.00098,
Bismuth 0.00099,
Palladium 0.001,
Selenium 0.00088,
Tellurium 0.0009,
Zinc 0.00098,
The silver matrix surplus.
4, standard pattern of emission spectrum of pure silver as claimed in claim 1 is characterized in that being made by following raw material by weight percentage:
Gold 0.0020,
Copper 0.0049,
Iron 0.0026,
Lead 0.0051,
Antimony 0.0021,
Bismuth 0.0021,
Palladium 0.0021,
Selenium 0.0019,
Tellurium 0.00199,
Zinc 0.0021,
The silver matrix surplus.
5, standard pattern of emission spectrum of pure silver as claimed in claim 1 is characterized in that being made by following raw material by weight percentage:
Gold 0.0039,
Copper 0.0106,
Iron 0.0049,
Lead 0.0104,
Antimony 0.0043,
Bismuth 0.0042,
Palladium 0.004,
Selenium 0.0039,
Tellurium 0.00387,
Zinc 0.0041,
The silver matrix surplus.
6, standard pattern of emission spectrum of pure silver as claimed in claim 1 is characterized in that being made by following raw material by weight percentage:
Gold 0.0081,
Copper 0.0199,
Iron 0.0099,
Lead 0.0206,
Antimony 0.0082,
Bismuth 0.0081,
Palladium 0.0079,
Selenium 0.0077,
Tellurium 0.0079,
Zinc 0.0079,
The silver matrix surplus.
7,, it is characterized in that comprising the steps: as the preparation method of the described standard pattern of emission spectrum of pure silver of one of claim 1～6
1), the selection of raw material: selecting silver content for use is that 99.995% fine silver is a silver matrix, and other metal selects for use tenor to be at least 99.9% simple metal;
2), batching: prepare burden in proportion;
3), founding: use medium-frequency induction furnace, after body of heater and the preheating of carbon crucible, add fine silver raw material and fusing earlier, then other raw material is added in the carbon crucible simultaneously, treat that fusing evenly and reach to take out rapidly behind 1100 ℃～1300 ℃ of the cast temperatures and adopt the combined type mold to cast promptly to make corresponding standard pattern of emission spectrum of pure silver.
8, the preparation method of standard pattern of emission spectrum of pure silver as claimed in claim 7 is characterized in that medium-frequency induction furnace adopts the 50KW medium-frequency induction furnace, and cast temperature is 1200 ℃.
9, the preparation method of standard pattern of emission spectrum of pure silver as claimed in claim 7, it is characterized in that described combined type mold comprises amalgamation successively and at least two moulds that connect by web member, above the mosaic between adjacent molds diversion groove is arranged, the plug hole that is communicated with diversion groove.
10, the preparation method of standard pattern of emission spectrum of pure silver as claimed in claim 9 is characterized in that pilot hole is arranged on the mold.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105928754A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Preparation method for standard spectral sample and application of standard spectral sample |
| CN112210687A (en) * | 2020-10-14 | 2021-01-12 | 山东黄金冶炼有限公司 | Preparation method of gold standard sample |
-
2005
- 2005-05-20 CN CNB200510020915XA patent/CN100494958C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105928754A (en) * | 2016-04-19 | 2016-09-07 | 攀钢集团研究院有限公司 | Preparation method for standard spectral sample and application of standard spectral sample |
| CN112210687A (en) * | 2020-10-14 | 2021-01-12 | 山东黄金冶炼有限公司 | Preparation method of gold standard sample |
| CN112210687B (en) * | 2020-10-14 | 2021-07-09 | 山东黄金冶炼有限公司 | Preparation method of gold standard sample |
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| CN100494958C (en) | 2009-06-03 |
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Assignee: The Great Wall Gold & Silver Refinery Assignor: CHINA BANKNOTE PRINTING AND MINTING Corp. Contract record no.: 2011510000337 Denomination of invention: Standard pattern of emission spectrum of pure silver, and preparation method Granted publication date: 20090603 License type: Exclusive License Open date: 20051116 Record date: 20111229 |
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Address after: 611130 Chengdu 0 District, Wenjiang 54 Sichuan three factory technical and quality office Patentee after: China Banknote Printing and Minting Group Co.,Ltd. Address before: 611130 Chengdu 0 District, Wenjiang 54 Sichuan three factory technical and quality office Patentee before: CHINA BANKNOTE PRINTING AND MINTING Corp. |
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