CN85105500A - The rapid test method of gold content in the high-load gold sample - Google Patents
The rapid test method of gold content in the high-load gold sample Download PDFInfo
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- CN85105500A CN85105500A CN 85105500 CN85105500A CN85105500A CN 85105500 A CN85105500 A CN 85105500A CN 85105500 CN85105500 CN 85105500 CN 85105500 A CN85105500 A CN 85105500A CN 85105500 A CN85105500 A CN 85105500A
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Abstract
The invention provides a kind of assay method of measuring gold content in the high-load gold sample fast and accurately.This method is taked to have added certain excessive sodium chloride solution with chloroazotic acid heating for dissolving sample the time, takes low-temperature heat to be evaporated near doing in the operation, removes chlorine and unnecessary acid, saves neutralization and regulates the acidity formality, reaches accurate result.Have and measure fast, can finish the mensuration overall process about 30 minutes; Method is simple, as long as the simple glass instrument just can carry out; Accuracy of measurement height, error be less than ± 0.2%, and the silver that exists in the sample, copper, lead etc. are interference-free simultaneously, the experiment favorable reproducibility, and the gold sample of consumption such as can reclaim at advantage, and is very suitable to regular production analytical work.
Description
A kind of gold determination method that relates to, the improvement of gold content method in the indirect volumetric determination high-load of a kind of Mohr's salt-potassium dichromate gold sample of more specifically saying so.
In prior art, to the mensuration of gold content in the high-load gold sample, past gravimetric method and the volumetric methods of adopting more.Gravimetric determination accuracy height, but formality is miscellaneous, is not suitable for daily production analysis; The method of volumetric determination gold content is a lot, the optimal indirect volumetric method of Mohr's salt-potassium dichromate that adopts at last.This is the method for the mensuration high-load gold sample gold content of А В И Л О В (CA.54:13970i) proposition, but owing to have problems on the assay method, makes that the experiment reappearance is bad, and error is big.Inquiring into its reason mainly contains: (1), with aqua regia dissolution gold sample generates AuCl
3, under heating evaporation and irradiate light, can be decomposed into AuCl or Au, influenced the accuracy of measuring.(2), in the sample evaporation process, do not have the temperature of fine control sand bath when particularly closely dried, when temperature surpasses 188 ℃, AuCl
3Can be decomposed into AuCl and element gold, also influence the accuracy of measuring.(3), use NaHCO during to minimum volume when sample evaporation
3Or Na
2CO
3Acid that it is unnecessary that solution or ammoniacal liquor neutralize and adjusting acidity, this is the formality trouble not only, and when the acid amount adds excessively inadequately, causes gold hydroxide precipitation or colloid " Lei Jin " resolution of precipitate incomplete again, makes measurement result on the low side.(4) for making Au
3+Fully be reduced to metallic gold, А В И Л О В adopt to add the way of greatly excessive Mohr's salt, but this has used too many 0.05N potassium bichromate solution when causing again coming the remaining ferrous salt of residual titration with potassium dichromate afterwards, and is extremely inconvenient in operation.From the initial stage in the sixties, just extensively adopt large-scale expensive equipment to carry out the mensuration of gold content in the world.Instrumental analysis speed is fast, but error is bigger, and particularly for the high sample of gold content, error at measurment is bigger.And instrument involves great expense, and producing can not widespread usage.Though the potentiometric titration in the instrumental analysis also can obtain result more accurately, it is convenient to be not so good as volumetric method.The domestic most employing test stones of China are estimated gold content, though this method is easy, evaluated error is big, even the master craftsman who knows a thing or two, the error of results estimated is all greater than more than 1%, and particularly for those gold and golds filled of mixing copper, the error of estimation is bigger.
The purpose of this invention is to provide and a kind ofly can overcome the volumetric method fast and accurately that there is shortcoming in the said determination method to measure gold content in the high-load gold sample.It neither needs with any valuable instrument, and the formality of mensuration is simple and easy again, convenient, practical again a kind of method on producing.
The present invention realizes above-mentioned task by following solution.
Gold is dissolved in the chloroazotic acid, generates (AuCl in the presence of sodium chloride or potassium chloride
4)
-1Complex compound.
Sample solution after the dissolving is evaporated near doing under the low-temperature heat state that is no more than 140 ℃ (being preferably between 120～140 ℃), after removing chlorine and unnecessary acid, the water that directly adds certain volume is with the dissolving soluble compound, at this moment the solution pH value is about 1, finding speed is accelerated, the formality of neutralization and adjusting acidity has guaranteed the accuracy of measuring simultaneously after saving, and improves the reappearance of experiment.
Under constantly stirring, add certain excessive standard mohr salt solution (
Ferrous sulfate amine (NH
4)
2Fe(SO
4)
26H
2O), make Au
3+Be reduced to metallic gold, continue again to stir about half a minute, make it Au
3+Reduction fully.Remaining mohr salt solution is with the K of standard
2Cr
2O
7The solution back titration it, its reaction is as follows:
Add an amount of sulphur phosphorus acid mixture and indicator such as diphenylamine sulfonic acid sodium salt and show the terminal point of titration.According to the residual titration amount of Mohr's salt addition and potassium bichromate solution, calculate Au%.
In the following formula: V '
Fe2+--adds the volume (milliliter) of standard mohr salt solution
T
Fe2+/Au--standard mohr salt solution is to the titer (grams per milliliter) of gold
W
Sample-weigh the weight (gram) of golden sample
In order to overcome the influence of chlorine residual in the said determination method to the measurement result accuracy, the present invention adopts three kinds of approach to solve.
(1), after sample dissolution is complete, under the low-temperature heat state, be evaporated to nearly do (preventing local overheating), after the cooling, wash wall of cup and watch glass once with an amount of concentrated hydrochloric acid solution, under the heated condition of low temperature control, be evaporated to nearly do (and preventing local overheating) again, after the cooling, add suitable quantity of water, make the soluble compound dissolving, add certain excessive standard mohr salt solution again, with standard weight potassium chromate solution residual titration it.Can access result accurately like this.
(2), adopt high pure gold (content is 99.999% or 99.99%) sample to obtain measured value by the said determination step, demarcate the N of potassium bichromate solution, also can obtain result accurately.
(3), the present invention adopts high pure gold (is 99.999% as content) sample to record result's absolute error as corrected value by the said determination step, when calculating gold content, deduct this corrected value, this method can also can obtain result accurately hurry up on finding speed.
According to the method for gold content in the mensuration high-load gold sample provided by the invention, be the indirect volumetric method of a kind of improved Mohr's salt-potassium dichromate.It is fast that this law has finding speed, and whole mensuration process just can be finished about 30 minutes; Accuracy of measurement height, the absolute error of mensuration be≤± 2 ‰; Measure simple procedure, do not need special instrument, as long as common glass apparatus can carry out, impurity such as the silver that exists in the sample, copper, aluminium do not disturb the mensuration of gold simultaneously, do not need to separate; The experiment favorable reproducibility; Grasp easily, if possess just, the people of senior middle school's schooling through short-term (3 thoughtful 1 month) training just can grasp; The gold sample that is consumed in experiment can reclaim or the like advantage, is highly suitable for regular production analytical work.
Be a most preferred embodiment of the present invention below:
Accurately weigh 0.18 gram (being accurate to 0.0001 gram) high-load gold sample (gold ornaments or Jin Jinjin) in 150 ml beakers, add 4 milliliters of chloroazotic acid, heating for dissolving in sand bath, after sample dissolution is complete, add 1 milliliter of low temperature in sand bath of 20% sodium chloride solution (120～140 ℃) immediately and be evaporated to nearly do (and preventing local overheating), watch glass and wall of cup are washed with 20 ml waters in the cooling back, under constantly stirring, add 50 milliliters of Mohr's salt standard solution lentamente exactly, continue again to stir half a minute, 15 milliliters in the sulphur phosphorus acid mixture that adds 1: 1: 3.5,5 of 30 milliliters in water and 0.5% diphenylamine sulfonic acid sodium salt indicator, becoming aubergine to solution from bottle green with the titration of standard weight potassium chromate solution immediately is terminal point.Calculate the percentage composition of gold, add corrected value, just obtain the content Au% of gold in the sample accurately.
Following table is the result that records with embodiments of the invention
The checking method that sample adopted and record Au% and record Au% with embodiments of the invention
No. 1 gold BEAMISH
*Gravimetric method records 91.5
Sample 91.7 91.7
91.8
91.8
91.6
No. 2 gold BEAMISH
*Gravimetric method records 96.0
Sample 95.9 96.0
95.9
96.1
No. 3 gold BEAMISH
*Gravimetric method records 91.8
Sample 91.7 91.8
(goldleaf) 91.9
No. 4 gold through Fujian Measuring Technology Inst. with 96.4
The sample plasma spectroscopy records 96.4
(gold plaque) 96.6
＊BEAMISH F.E.ET AL.，IND.ENG.CHEM.，ANAL.ED.，9 174-5（1937）
Find out from last table, can record satisfied result with method of the present invention.
Claims (5)
1, a kind of method of fast, accurately measuring gold content in the high-load gold sample, its step comprises with chloroazotic acid heating for dissolving sample, after being evaporated near doing, add excessive standard mohr salt solution, use again standard weight potassium chromate solution residual titration it, according to standard mohr salt solution addition and standard weight potassium chromate solution residual titration amount, the gold content of calculation sample the invention is characterized in:
(A), sample with the chloroazotic acid heating for dissolving fully after, add certain excessive sodium chloride or Klorvess Liquid immediately, make Au
3+Form stable [AuCl
4]
-1Complex compound.
(B), in the good sample evaporation process of dissolving, the temperature in the strict control sand bath allows sample be evaporated near doing under the state of low-temperature heat, to remove chlorine and unnecessary acid.
(C), do near, after the cooling, add suitable quantity of water when sample evaporation, make the soluble compound dissolving after, under constantly stirring, accurately add certain excessive mohr salt solution lentamente after, continue to stir about half a minute, make Au
3+By Fe
2+Be reduced to metallic gold fully, use again standard weight potassium chromate solution residual titration it.
2,, it is characterized in that adopting absolute error that high pure gold (is 99.999% as content) records gained as a result as corrected value, the error that occurs in order to influenced by residual chlorine according to the described determination method of claim 1.
3, according to the described assay method of claim 1, it is characterized in that after sample dissolution is complete, under the state of low-temperature heat, be evaporated near doing, after the cooling, with an amount of concentrated hydrochloric acid solution washing wall of cup and watch glass once, under the state of low-temperature heat, be evaporated near doing again, after the cooling, add suitable quantity of water and make the soluble compound dissolving, with method titration by measure between standard Mohr's salt-potassium bichromate solution it, to obtain accurate measured value.
4, according to the described assay method of claim 1, the N that the result who it is characterized in that adopting high pure gold (is 99.999% as content) to measure by the sample determination formality demarcates potassium bichromate solution is with the exact value that obtains to measure.
5, according to claim 1,3 described assay methods is characterized in that dissolving good sample in being evaporated to the nearly process of doing, and the temperature in the control sand bath is no more than 140 ℃, generally is advisable with 120 ℃～140 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105500 CN85105500A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in the high-load gold sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105500 CN85105500A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in the high-load gold sample |
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| Publication Number | Publication Date |
|---|---|
| CN85105500A true CN85105500A (en) | 1987-01-14 |
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ID=4794518
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85105500 Pending CN85105500A (en) | 1985-07-15 | 1985-07-15 | The rapid test method of gold content in the high-load gold sample |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102252935A (en) * | 2011-04-07 | 2011-11-23 | 广西地博矿业集团股份有限公司 | Chemical gravimetric method for determining content of gold in gold-loaded carbon |
| CN101046453B (en) * | 2007-04-24 | 2012-04-25 | 青海西部矿业科技有限公司 | Iodometry process of measuring gold content in high accuracy and precision |
| CN103575609A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing gold in liquid gold water |
| CN109813835A (en) * | 2017-11-22 | 2019-05-28 | 中国瑞林工程技术股份有限公司 | The method for measuring gold and silver content in useless circuit board |
| CN111089934A (en) * | 2020-01-13 | 2020-05-01 | 南京市产品质量监督检验院 | Method for measuring cyanide content in gold product by using ion chromatography technology |
| CN112504906A (en) * | 2020-11-12 | 2021-03-16 | 昆山全亚冠环保科技有限公司 | Analysis and quantification method for total carbon in gold material |
-
1985
- 1985-07-15 CN CN 85105500 patent/CN85105500A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101046453B (en) * | 2007-04-24 | 2012-04-25 | 青海西部矿业科技有限公司 | Iodometry process of measuring gold content in high accuracy and precision |
| CN102252935A (en) * | 2011-04-07 | 2011-11-23 | 广西地博矿业集团股份有限公司 | Chemical gravimetric method for determining content of gold in gold-loaded carbon |
| CN103575609A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing gold in liquid gold water |
| CN103575609B (en) * | 2013-11-07 | 2015-07-01 | 广州有色金属研究院 | Method for analyzing gold in liquid gold water |
| CN109813835A (en) * | 2017-11-22 | 2019-05-28 | 中国瑞林工程技术股份有限公司 | The method for measuring gold and silver content in useless circuit board |
| 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 |
| CN111089934A (en) * | 2020-01-13 | 2020-05-01 | 南京市产品质量监督检验院 | Method for measuring cyanide content in gold product by using ion chromatography technology |
| CN112504906A (en) * | 2020-11-12 | 2021-03-16 | 昆山全亚冠环保科技有限公司 | Analysis and quantification method for total carbon in gold material |
| CN112504906B (en) * | 2020-11-12 | 2022-06-14 | 光洋新材料科技(昆山)有限公司 | Analysis and quantification method for total carbon in gold material |
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