CN108562512A - A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery - Google Patents

A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery Download PDF

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Publication number
CN108562512A
CN108562512A CN201810695741.4A CN201810695741A CN108562512A CN 108562512 A CN108562512 A CN 108562512A CN 201810695741 A CN201810695741 A CN 201810695741A CN 108562512 A CN108562512 A CN 108562512A
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Prior art keywords
gold
sample
standard
cupel
rolled
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赫婷婷
那勃
孟建华
曹维宇
张伟桃
崔建军
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TIANJIN PRODUCT QUALITY SUPERVISION AND TESTING INSTITUTE
Huajin National Inspection (shenzhen) Gold And Silver Jewelry Inspection Center Co Ltd
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TIANJIN PRODUCT QUALITY SUPERVISION AND TESTING INSTITUTE
Huajin National Inspection (shenzhen) Gold And Silver Jewelry Inspection Center Co Ltd
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Priority to CN201810695741.4A priority Critical patent/CN108562512A/en
Publication of CN108562512A publication Critical patent/CN108562512A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The present invention relates to a kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery, this method is added suitable gold and silver in sample, receipts agent is flutterred with lead, is placed in porosity cupel and carries out oxidation ash and blow.Lead oxides and impurity are absorbed by cupel, and it is noble metal ball that gold and silver, which are trapped in melting,.It is rolled into thin slice and is rolled into rouleau, be placed in nitric acid, after silver is gradually dissolved, obtain the quality of gold.It is proposed by the present invention to add golden method, it can all greatly improve the accuracy of experiment, the collimation of data detects work for daily noble metal jewelry and brings convenience, and ensures detection everything goes well with your work satisfactory complete.

Description

A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery
Technical field
The present invention relates to the detection method of the main amount of gold more particularly to a kind of Fire Assayings in karat gold jewellery to add golden method detection karat gold head The method of gold content in decorations.
Background technology
With the continuous improvement of people's living standards, noble metal jewelry is increasingly liked by consumers in general, especially It is the noble metal jewelry of white.Currently, white noble metal jewelry mainly has platinum alloy, palldium alloy and karat gold alloy first in the market Decorations.The main component of preceding 2 kinds of jewellery is respectively Pt and Pd, belongs to Pt races element, itself is white;Karat gold alloy is in gold Pd or Ni etc. is added, keeps its white or light yellow.Karat gold hardness is high, toughness is small, brightness is high, is unlikely to deform, not easy to wear, valence Lattice relative moderate, workmanship is careful, and appearance is salubrious, any surface finish, and interior light sensation is strong, therefore has obtained widely applying.
In China, white karat gold alloy jewellery other than Au, it is mainly added with Ag, Ni, Cu etc., and it is international, it leads Add Pd, Cu, Ag etc..Precisely due to karat gold formula in metallic element variability, cause the difficulty of detection, China fire Ensaying method is the referee method in GB11887, but common fire assaying to the detection of low content karat gold (such as 14K gold, 9K gold) also It is to have certain difficulty.If nickel in karat gold jewellery, Zn-ef ficiency content is higher, electrum gold volume quality can be caused crisp, in parting Cause in the process gold roll up crushing, it is scaling-off phenomena such as, and then influence final result.It is based on fire assaying in the prior art Deficiency, the present invention provides a kind of Fire Assayings to add the method that golden method measures gold content in karat gold jewellery, has compensated for the prior art In deficiency, improve the accuracy of measurement.
Invention content
The purpose of the present invention is to provide a kind of methods that Fire Assaying adds gold content in golden method detection karat gold jewellery, can be significantly Deficiency in the prior art is compensated for, the accuracy of measurement is improved.
In order to achieve the above objectives, the present invention adopts the following technical scheme that, a kind of Fire Assaying adds to be contained in golden method detection karat gold jewellery The method of gold amount, it includes following steps:
(1) it weighs
The standard gold and sample for weighing 200-320mg phase homogenous quantities, are accurate to 0.01mg, are surveyed respectively with X fluorescence spectrum survey Go out the gold content in standard gold and in sample, a certain proportion of standard gold is added in the sample, the mark for being allowed to gold content and weighing Gold content is suitable in quasi- gold, and the mark for being equivalent to 2.5-3 times of standard gold quality is then added in the standard gold and sample weighed Quasi- silver;Load weighted standard gold and sample are wrapped with lead foil respectively, are rolled into ball sample;
(2) ash is blown
Standard gold that lead foil wraps is placed in sample in cupel(lation) furnace with long handle stainless pucellas be preheated to 980 DEG C- In 1100 DEG C of cupel, standard gold and sample cross are arranged, cause error, furnace temperature to be maintained at 980 to avoid furnace temperature is uneven DEG C -1100 DEG C, under oxidative conditions, continuous heating is completely melt until sample;
(3) annealing roller sheet
700 DEG C are cooled the temperature to hereinafter, standard gold and sample are taken out from cupel with tweezers and brush away attachment with brush In cupel material above, it is put into iron and pricks on son, clamp and use hammer rectangularity, and anneal, rolled into flaking machine The thin slice of 0.15mm-0.2mm is annealed, cooling, is rolled into cylindrical shape;
(4) parting
Gold volume is immersed in and fills 100ml, in the parting basket for closely boiling nitric acid (1+1), is allowed to remain at the temperature closely boiled The lower 10-30min of degree, catches up with most nitrogen oxides, parting basket is taken out, and clean gold with 60 DEG C of -70 DEG C of hot water and rolls up 3-5 times, then again The parting basket for filling gold volume is put into the nitric acid (2+1) closely boiled, boils 10-15min, is taken out and is washed 3-5 with 60 DEG C of -70 DEG C of hot water It is secondary;
By standard gold and the sample drying on electric furnace after parting, it is then placed in 700 DEG C of -750 DEG C of heating 3- in Muffle furnace 6min, it is cooling, gold volume quality is weighed, 0.01mg is accurate to.
Further, the lead foil weight is 2-4g.
Further, cupric in sample, nickel, zinc amount are measured with X fluorescence spectrum, be added in standard gold in sample Cupric, nickel, the comparable copper of zinc amount, nickel, zinc.
Suitable golden (to increase the toughness of gold volume, preferably parting is prepared for energy) and silver is added in sample in the present invention, Flutter receipts agent with lead, be placed in porosity cupel carry out oxidation ash blow.Lead oxides and impurity are absorbed by cupel, and gold and silver are stagnant It is noble metal ball to stay in melting.It is rolled into thin slice and is rolled into rouleau, be placed in nitric acid, after silver is gradually dissolved, obtain gold Quality.Analysis comparison is carried out using standard gold simultaneously, the systematic error in analytic process can be eliminated.It is proposed by the present invention to add gold Method, can all greatly improve the accuracy of experiment, and the collimation of data detects work for daily noble metal jewelry and brings convenience, protects Everything goes well with your work satisfactory completes for card detection.
Specific implementation mode
It is more clear clear to make the objectives, technical solutions, and advantages of the present invention seem, now passes through specific embodiment pair The present invention is further explained explanation.
Embodiment
A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery, it includes following steps:
(1) it weighs
The standard gold and sample for weighing phase homogenous quantities are surveyed the gold content measured respectively in standard gold with X fluorescence spectrum, are being tried A certain proportion of standard gold is added in sample, it is suitable with gold content in the standard gold weighed to be allowed to gold content, then in the mark weighed The standard silver for being equivalent to 2.5 times of standard gold quality is added in quasi- gold and sample;Load weighted standard gold and sample are used respectively Lead foil is wrapped, and ball sample is rolled into;
(2) ash is blown
The standard gold that lead foil wraps is placed in sample with long handle stainless pucellas and is preheated to 980 DEG C in cupel(lation) furnace In cupel, standard gold and sample cross are arranged, causes error, furnace temperature to be maintained at 980 DEG C to avoid furnace temperature is uneven, is aoxidizing Under the conditions of, continuous heating is completely melt until sample;
(3) annealing roller sheet
700 DEG C are cooled the temperature to hereinafter, standard gold and sample are taken out from cupel with tweezers and brush away attachment with brush In cupel material above, it is put into iron and pricks on son, clamp and use hammer rectangularity, and anneal, rolled into flaking machine The thin slice of 0.15mm or so is annealed, cooling, is rolled into cylindrical shape;
(4) parting
Gold volume is immersed in and fills 100ml, in the parting basket for closely boiling nitric acid (1+1), is allowed to remain at the temperature closely boiled The lower 10min of degree, catches up with most nitrogen oxides, parting basket is taken out, and gold volume clean 3 times with 60 DEG C of hot water, then again filling what gold was rolled up Parting basket is put into the nitric acid (2+1) closely boiled, boils 15min, and taking-up is washed 3 times with 60 DEG C of hot water;
By standard gold and the sample drying on electric furnace after parting, it is then placed in Muffle furnace and heats 5min for 700 DEG C, it is cold But, gold volume quality is weighed, 0.01mg is accurate to.
It is respectively that 18K is golden (Huang), 18K gold (white-nickeliferous), 14K gold (Huang), 14K gold (yellow-to contain zinc), 9K gold (Huang), 9K gold (white) to be tested using above-described embodiment method, specific experimental condition is as follows:
Comparative example
A kind of method that fire assaying detects gold content in karat gold jewellery, it includes following steps:
(1) it weighs
The standard gold and sample for weighing phase homogenous quantities weigh identical quality according to the quality with sample in above-described embodiment Sample and standard gold;Load weighted standard gold and sample are wrapped with lead foil respectively, are rolled into ball sample;
(2) ash is blown
The standard gold that lead foil wraps is placed in sample with long handle stainless pucellas and is preheated to 980 DEG C in cupel(lation) furnace In cupel, standard gold and sample cross are arranged, causes error, furnace temperature to be maintained at 980 DEG C to avoid furnace temperature is uneven, is aoxidizing Under the conditions of, continuous heating is completely melt until sample;
(3) annealing roller sheet
700 DEG C are cooled the temperature to hereinafter, standard gold and sample are taken out from cupel with tweezers and brush away attachment with brush In cupel material above, it is put into iron and pricks on son, clamp and use hammer rectangularity, and anneal, rolled into flaking machine The thin slice of 0.15mm is annealed, cooling, is rolled into cylindrical shape;
(4) parting
Gold volume is immersed in and fills 100ml, in the parting basket for closely boiling nitric acid (1+1), is allowed to remain at the temperature closely boiled The lower 10min of degree, catches up with most nitrogen oxides, parting basket is taken out, and gold volume clean 3 times with 60 DEG C of hot water, then again filling what gold was rolled up Parting basket is put into the nitric acid (2+1) closely boiled, boils 15min, and taking-up is washed 3 times with 60 DEG C of hot water;
By standard gold and the sample drying on electric furnace after parting, it is then placed in Muffle furnace and heats 5min for 700 DEG C, it is cold But, gold volume quality is weighed, 0.01mg is accurate to.
Test result is as follows shown in table:
According to upper table as can be seen that the common fire assaying of yellow 18K gold and adding the collimation of golden method testing result and trying out Property gap is little;The collimation that nickeliferous white 18K gold adds golden method institute measured data is better than common fire assaying.Huang without zinc Color 14K gold adds golden method institute measured data collimation and is better than common fire assaying;Huang, white 14K gold containing zinc add golden method whether The actual operation of experiment or the collimation of the integrality of final sample and data will be higher than common fire assaying.It is yellow, white The collimation for the integrality and data that 9K gold adds the actual operation that golden method is whether tested or final sample will be higher than general Logical fire assaying.So the property on probation that karat gold jewellery add golden method is higher than common fire assaying.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (3)

1. a kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery, which is characterized in that this method includes following step Suddenly:
(1)It weighs
The standard gold and sample for weighing 200-320mg phase homogenous quantities, are accurate to 0.01mg, and standard is measured respectively with X fluorescence spectrum Gold neutralizes the gold content in sample, and a certain proportion of standard gold is added in the sample, is allowed in gold content and the standard gold that weighs Gold content is suitable, and the standard silver for being equivalent to 2.5-3 times of standard gold quality is then added in the standard gold and sample weighed;It will Load weighted standard gold and sample are wrapped with lead foil respectively, are rolled into ball sample;
(2)Ash is blown
The standard gold that lead foil wraps is placed in sample in cupel(lation) furnace with long handle stainless pucellas and is preheated to 980 DEG C -1100 DEG C cupel in, standard gold and sample cross are arranged, error is caused to avoid furnace temperature is uneven, furnace temperature be maintained at 980 DEG C- 1100 DEG C, under oxidative conditions, continuous heating is completely melt until sample;
(3)Annealing roller sheet
700 DEG C are cooled the temperature to hereinafter, standard gold and sample are attached to from taking out in cupel and brushed away with brush with tweezers The cupel material in face is put into iron and pricks on son, clamps and use hammer rectangularity, and anneal, 0.15mm- is rolled into flaking machine The thin slice of 0.2mm is annealed, cooling, is rolled into cylindrical shape;
(4)Parting
Gold volume is immersed in and fills 100ml, closely boils nitric acid(1+1)Parting basket in, at a temperature of being allowed to remain at nearly boiling 10-30min catches up with most nitrogen oxides, parting basket is taken out, and gold volume is cleaned 3-5 times with 60 DEG C of -70 DEG C of hot water, then again filling The parting basket of gold volume is put into the nitric acid closely boiled(2+1)In, 10-15min is boiled, taking-up is washed 3-5 times with 60 DEG C of -70 DEG C of hot water;
By standard gold and the sample drying on electric furnace after parting, 700 DEG C of -750 DEG C of heating 3-6min in Muffle furnace are then placed in, It is cooling, gold volume quality is weighed, 0.01mg is accurate to.
2. according to the method described in claim 1, it is characterized in that, the lead foil weight is 2-4g.
3. according to the method described in claim 1, it is characterized in that, being also added into standard gold and cupric, nickel, zinc in sample Measure comparable copper, nickel, zinc.
CN201810695741.4A 2018-06-29 2018-06-29 A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery Pending CN108562512A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109540731A (en) * 2019-01-15 2019-03-29 长春黄金研究院有限公司 A kind of silver determination method in electrolysis cathode steel wool
CN109580419A (en) * 2018-11-06 2019-04-05 长春黄金研究院有限公司 Golden measuring method in a kind of cathode steel wool of electrodeposition gold
CN109856006A (en) * 2018-12-26 2019-06-07 励福(江门)环保科技股份有限公司 A kind of method of multiple element content in efficient detection karat gold
CN112630088A (en) * 2020-12-28 2021-04-09 国家珠宝检测中心(广东)有限责任公司 Low-purity gold quantitative detection method
CN113376145A (en) * 2021-08-16 2021-09-10 北矿检测技术有限公司 Method for measuring amount of palladium in copper matte
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
CN115753277A (en) * 2022-11-04 2023-03-07 山东招金金银精炼有限公司 Method for analyzing gold content in high-copper-content alloy gold

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109580419A (en) * 2018-11-06 2019-04-05 长春黄金研究院有限公司 Golden measuring method in a kind of cathode steel wool of electrodeposition gold
CN109856006A (en) * 2018-12-26 2019-06-07 励福(江门)环保科技股份有限公司 A kind of method of multiple element content in efficient detection karat gold
CN109540731A (en) * 2019-01-15 2019-03-29 长春黄金研究院有限公司 A kind of silver determination method in electrolysis cathode steel wool
CN112630088A (en) * 2020-12-28 2021-04-09 国家珠宝检测中心(广东)有限责任公司 Low-purity gold quantitative detection method
CN113899653A (en) * 2020-12-28 2022-01-07 国家珠宝检测中心(广东)有限责任公司 Low-purity gold quantitative detection method
CN113899653B (en) * 2020-12-28 2022-09-13 国家珠宝检测中心(广东)有限责任公司 Low-purity gold quantitative detection method
CN113376145A (en) * 2021-08-16 2021-09-10 北矿检测技术有限公司 Method for measuring amount of palladium in copper matte
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
CN115753277A (en) * 2022-11-04 2023-03-07 山东招金金银精炼有限公司 Method for analyzing gold content in high-copper-content alloy gold

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