CN100529723C - Method for detecting high content gold by fire assaying - Google Patents
Method for detecting high content gold by fire assaying Download PDFInfo
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- CN100529723C CN100529723C CNB2006101246678A CN200610124667A CN100529723C CN 100529723 C CN100529723 C CN 100529723C CN B2006101246678 A CNB2006101246678 A CN B2006101246678A CN 200610124667 A CN200610124667 A CN 200610124667A CN 100529723 C CN100529723 C CN 100529723C
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Abstract
The fire assaying method for detecting high content gold includes the following steps: rolling the sample into foil, adding 2.5 times Ag and Cu in 50 mg, wrapping in lead foil and forming into ball; setting the tested sample and the gold standard in cupel and cupelling; tapping to form oblate, rolling into sheet, winding into hollow reels and setting into parting basket; heating in water bath for parting for three times, stoving in a stove for 15 min, setting in ceramic crucible, annealing at 800 deg.c for 5 min, weighing and calculating. The fire assaying method of the present invention has high accuracy.
Description
Technical field
The present invention relates to the assay method of the main amount of gold in the ingot, especially a kind of method of detecting high content gold by fire assaying.
Background technology
The analytical approach of gold mainly contains three kinds in the current mensuration ingot: fire assaying, spectrum decrement determination method and chemical decrement determination method.Spectrum decrement determination method and chemical decrement determination method all only are applicable to measures the ingot contain Au＞99.95%, for Au＜99.95% because impurity content height, impurity element kind are measured not congruent reason, cause the accuracy variation of measurement result and inapplicable.And fire assaying is directly to measure main amount gold, be not subjected to the impurity quantitative limitation, fire assaying can be removed impurity element effectively because of it, thereby the accuracy of measurement result is higher, but the national standard method GB/T 15249-1994 of present fiery ensaying gravimetric determination gold amount, because of its to the analytic process and the reasons such as standard sample line purity is not enough that adopt, make its accuracy and precision all not reach optimum, stipulate in the method that Au＞99.5% franchise is 0.0002%, in fact be difficult to realize, with international most advanced level 99.5%＜Au＜99.95% franchise be 0.00015%, Au＞99.95% franchise is 0.00005%, and tangible gap is arranged.
Summary of the invention
Purpose of the present invention just provides a kind of method of detecting high content gold by fire assaying, and this method can improve the accuracy and the precision of measurement result.
The method of detecting high content gold by fire assaying of the present invention is:
1, the testing sample removing surface is clean, grind flakiness, replace weighing testing sample and goldstandard with balance, put into ready lead foil, in every part of goldstandard and testing sample, add the fine silver and the 50mg fine copper of 2.5 times of gold amounts, be rolled into sphere with sheet lead;
2, cupel is put into 950 ± 10 ℃ cupel(lation) furnace preheating 30 minutes, then above-mentioned testing sample that has added fine silver, fine copper and the goldstandard that has added fine silver, fine copper are put into cupel in order, close fire door, treat that test portion is all after the fusing, the blow-on door carries out ash and blows slightly, until grey blowing bundle;
3, close grain, rap and close a both sides, make it to be oblate, brush away attachment, in 800 ℃ of annealing 5 minutes, taking-up will be closed grain and be ground flakiness, gold and silver be closed a thin slice again and be rolled into two reverse coreless rolls, put into parting basket successively by the ash mode of blowing, and use hot wash;
4, carry out parting three times with water-bath heating, when nitric acid was heated to 80-85 ℃ in 1: 1, parting basket put into begins to carry out parting, parting 40 minutes takes out with after the hot wash; Put into 2: 1 nitric acid partings again 30 minutes, and took out with after the hot wash; Put into 2: 1 nitric acid partings again 30 minutes; Taking-up with hot wash after, parting basket is put into 105 ℃ baking oven baking 15 minutes, take out, with tweezers the gold volume is moved in the porcelain crucible, in 800 ℃ of annealing 5 minutes, take out cooling, on microbalance, weigh, calculate.
The calculating of analysis result and statement:
The percentage composition of the gold of testing sample is calculated as follows:
In the formula: m
1---testing sample gold volume quality, g;
m
2---the quality of testing sample, g;
m
3---goldstandard gold volume quality, g;
m
4---the quality of goldstandard, g;
D---the percentage composition of goldstandard gold.
In said method, goldstandard is done standard with the High Purity Gold of gold content＞99.999% and is used, the fine copper that adds is blown over the fusing point that reduces gold in the journey at ash, prevents golden oxidation, can avoid gold and silver to close grain adsorbed gas in temperature-fall period and discharge too fast and occur splashing and make the gold loss.
Adopted exclusive protective agent copper in the method for detecting high content gold by fire assaying of the present invention; and to all details of operation all in addition optimization and standard; can reach the pin-point accuracy high precision; franchise can be controlled the world level of advancing; 99.5%＜Au＜99.95% franchise is 0.00015%, and Au＞99.95% franchise is 0.00005%.
Embodiment
It is 99.85% that two ingot prediction gold contents are arranged.
Sample surfaces is cleaned out, grind flakiness again, replace weighing with balance and treat each four parts of test samples and five parts of goldstandards (Au＞99.999%), accurately to 0.0000001g, goldstandard sample amount is controlled in 0.5000000～0.5005000g, and testing sample sample amount is controlled in 0.5005000～0.5010000g, puts into ready lead foil, the lead foil general assembly (TW) is about in 11.6 ± 0.1g, finishes in 1 hour.Every part of goldstandard with treat to add in the test sample 1.250 ± 0.001g fine silver and 50mg fine copper, sheet lead is rolled into sphere.Cupel is put into 950 ± 10 ℃ of cupel(lation) furnace preheatings 30 minutes, will treat that then test sample and goldstandard put into cupel in order, close fire door, treat test portion all after the fusing, the blow-on door carries out ash and blows slightly, until grey blowing bundle.Take out gold and silver and close grain, rap and close a both sides, make it to be oblate, brush away attachment.800 ℃ of annealing 5 minutes, taking-up will be closed grain and be ground into the length and width of 0.12 ± 0.02mm, thick basically identical thin slice, annealed 5 minutes at 800 ℃, the gold and silver after the annealing is closed be rolled into two reverse coreless rolls after a thin slice cools off, put into parting basket successively by the ash mode of blowing.Parting three times, for the first time parting: parting basket put into be preheated to 85 ℃ 1: 1 nitric acid with water-bath and begin parting, parting 40 minutes takes out the parting basket hot wash; Parting for the second time: the parting basket after will wash was placed in the water-bath in enough long 2: 1 nitric acid of preheating parting 30 minutes, the hot wash of taking-up parting basket; Parting is from multiple operation for the second time for the third time.The baking oven that parting basket after washing is put into 105 ℃ dried by the fire 15 minutes, took out, and the gold volume is taken out from parting basket put into porcelain crucible successively, annealed 5 minutes in 800 ℃ cupel(lation) furnace then, weighed on microbalance and calculate in taking-up cooling back.
Claims (2)
1, a kind of method of detecting high content gold by fire assaying, it is characterized in that: it may further comprise the steps:
(1), the testing sample removing surface is clean, grind flakiness, replace weighing testing sample and goldstandard with balance, put into ready lead foil, in every part of goldstandard and testing sample, add fine silver and the 50mg fine copper that 2.5 times of gold are measured, be rolled into sphere with sheet lead;
(2), cupel is put into 950 ± 10 ℃ cupel(lation) furnace preheating 30 minutes, then above-mentioned testing sample that has added fine silver, fine copper and the goldstandard that has added fine silver, fine copper are put into cupel in order, close fire door, after treating that test portion all melts, the blow-on door carries out ash and blows slightly, until grey blowing bundle;
(3), close grain, rap and close a both sides, make it to be oblate, brush away attachment, in 800 ℃ of annealing 5 minutes, taking-up will be closed grain and be ground flakiness, again gold and silver is closed a thin slice and be rolled into two reverse coreless rolls, put into parting basket successively by the ash mode of blowing, and use hot wash;
(4), carry out parting three times, when nitric acid was heated to 80-85 ℃ in 1: 1, parting basket put into begins to carry out parting, parting 40 minutes takes out with after the hot wash with water-bath heating; Put into 2: 1 nitric acid partings again 30 minutes, and took out with after the hot wash; Put into 2: 1 nitric acid partings again 30 minutes; Taking-up with hot wash after, parting basket is put into 105 ℃ baking oven baking 15 minutes, take out, with tweezers the gold volume is moved in the porcelain crucible, in 800 ℃ of annealing 5 minutes, take out cooling, on microbalance, weigh;
The percentage composition of the gold of testing sample is calculated as follows:
In the formula: m
1---testing sample gold volume quality, g;
m
2---the quality of testing sample, g;
m
3---goldstandard gold volume quality, g;
m
4---the quality of goldstandard, g;
D---the percentage composition of goldstandard gold.
2, the method for detecting high content gold by fire assaying according to claim 1 is characterized in that: described goldstandard is the High Purity Gold of gold content＞99.999%.
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| CNB2006101246678A CN100529723C (en) | 2006-09-28 | 2006-09-28 | Method for detecting high content gold by fire assaying |
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| CNB2006101246678A CN100529723C (en) | 2006-09-28 | 2006-09-28 | Method for detecting high content gold by fire assaying |
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| CN1945273A CN1945273A (en) | 2007-04-11 |
| CN100529723C true CN100529723C (en) | 2009-08-19 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493395B (en) * | 2008-01-24 | 2011-03-30 | 中山火炬职业技术学院 | Method for measuring rhodium content in plating liquid |
| CN102128850B (en) * | 2010-12-08 | 2012-08-01 | 南京市产品质量监督检验院 | Method for quickly determining gold content of gold foil |
| CN102253072A (en) * | 2011-06-14 | 2011-11-23 | 白银有色集团股份有限公司 | Pyrometallurgical ensaying method for controlling quality of lead button |
| CN103115886A (en) * | 2013-01-30 | 2013-05-22 | 广州有色金属研究院 | Method for analyzing gold in tin and tin alloy waste |
| CN104458707A (en) * | 2014-12-07 | 2015-03-25 | 金川集团股份有限公司 | Method for separating silver in gold-palladium-platinum testing process |
| CN105547897A (en) * | 2016-01-26 | 2016-05-04 | 山东黄金矿业(莱州)有限公司精炼厂 | Method for jointly measuring content of gold and content of silver in cyanide gold mud |
| CN105651929B (en) * | 2016-03-02 | 2017-07-18 | 祝培明 | Intelligent Fire Assaying cupel(lation) furnace |
| CN105910950A (en) * | 2016-07-07 | 2016-08-31 | 长春黄金研究院 | Method for testing content of gold in crude silver by using fire assaying method |
| CN106124359A (en) * | 2016-07-08 | 2016-11-16 | 长春黄金研究院 | The assay method of silver amount in a kind of gold loaded carbon |
| CN109813835B (en) * | 2017-11-22 | 2021-10-26 | 中国瑞林工程技术股份有限公司 | Method for measuring gold and silver content in waste circuit board |
| CN108562512A (en) * | 2018-06-29 | 2018-09-21 | 华津国检（深圳）金银珠宝检验中心有限公司 | A kind of method that Fire Assaying adds gold content in golden method detection karat gold jewellery |
| CN109708991A (en) * | 2018-12-22 | 2019-05-03 | 励福(江门)环保科技股份有限公司 | A kind of novel fire assaying |
| CN110567838B (en) * | 2019-09-29 | 2021-05-07 | 珠海格力电器股份有限公司 | Method for detecting gold content in gold-plated part |
| CN112210687B (en) * | 2020-10-14 | 2021-07-09 | 山东黄金冶炼有限公司 | Preparation method of gold standard sample |
| CN113295573B (en) * | 2021-05-21 | 2024-01-16 | 深圳市金质金银珠宝检验研究中心有限公司 | Method for detecting gold content of electroformed hard gold product |
| CN115753277B (en) * | 2022-11-04 | 2023-07-21 | 山东招金金银精炼有限公司 | Analysis method for gold content in high-copper-content alloy |
-
2006
- 2006-09-28 CN CNB2006101246678A patent/CN100529723C/en active Active
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