CN101424635A - Aurum element analyzing and detecting method in smelting material - Google Patents
Aurum element analyzing and detecting method in smelting material Download PDFInfo
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- CN101424635A CN101424635A CNA2008102401152A CN200810240115A CN101424635A CN 101424635 A CN101424635 A CN 101424635A CN A2008102401152 A CNA2008102401152 A CN A2008102401152A CN 200810240115 A CN200810240115 A CN 200810240115A CN 101424635 A CN101424635 A CN 101424635A
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Abstract
The invention relates to a method for analyzing and detecting gold elements in smelting materials, which comprises the following steps: a sample is added into nitric acid or tartaric acid for heating pretreatment; the test solution is filtered by filter paper, and residue is fully transferred to the filter paper and is washed; the filter paper and the residue are put in a ceramic crucible and are put in a muffle furnace at a temperature of 750 DEG C for full incineration; fresh aqua fortis is added for dissolving and incinerating the residue at a low temperature; a combustion supporting ratio of 5:1, a slit of 0.2mm, a lamp current of 2mA and a negative high voltage of 300V are chosen, an atomic absorption spectrophotometer is used for determining the light absorption values of the gold elements, and results are calculated and analyzed. The method of the invention for analyzing the gold elements in the smelting materials has simplicity, convenience, easy implementation, short flow, small investment, high determination accuracy and good repeatability.
Description
Technical field
The present invention relates to the analyzing detecting method of gold element in the analyzing detecting method of gold element, particularly smelting material, it is applicable to the analyzing and testing of smelting material gold elements such as lead anode slurry, lead bismuth alloy, high silver-colored slag, lead bullion, thick bismuth, thick silver, blister copper.
Background technology
In the analyzing detecting method of existing gold element, the concentration and separation of the gold element process that is absolutely necessary, its means have varied: fire assaying, preconcentration with activated carbon partition method, polyfoam concentration and separation method, ion-exchange concentration and separation method etc.Because the equipment that these enrichment and separation methods need be expensive, special material and a large amount of chemical reagent, operating process is difficult to be grasped, and long flow path, labour intensity is big, measure gold element (standard GB/T7739.1-2007 Gold Concentrate under Normal Pressure chemical analysis method) as assaying of firing method and need expensive instrument and equipment such as assay furnace, cupel(lation) furnace, microbalance and a large amount of fusion reagent, analytic process is difficult for grasping, need certain practical experience, therefore, these analytical approachs are not that general assay office can be set up.
Summary of the invention
The analyzing detecting method that the purpose of this invention is to provide gold element in a kind of smelting material, overcome the defective of concentration and separation method in the above-mentioned gold element mensuration process, a kind of easy, easy row, the little gold element analyzing detecting method of investment are provided, to adapt to the analyzing and testing of gold element in the smelting material, the analysis result accuracy height, favorable reproducibility.
For realizing the object of the invention, adopted the nitric acid decomposition, isolated by filtration base metal and other impurity, the enrichment gold element after the aqua regia dissolution gold element, is carried out the technical scheme of analyzing and testing with Atomic Absorption Spectrometer, and concrete steps comprise:
(1) the smelting material sample is added nitric acid and tartrate, and carry out heating pretreatment;
(2) after the preprocessing solution cooling, use filter paper filtering, all be transferred on the filter paper residue and washing, make gold element and matrix bismuth, lead, silver and other separation of foreign elements;
(3) will wash good filter paper and residue and put into porcelain crucible, and place the interior ashing of muffle furnace complete;
(4) use the aqua regia dissolution ash content, be prepared into test solution to be measured;
(5) select combustion to help than 5:1, slit 0.2mm, lamp current 2mA, negative high voltage 300V is with atomic absorption spectrometry gold element light absorption value, Calculation results.
Preferably, during the heating pretreatment sample, concentration of nitric acid is 4mol/L, and tartrate is solid.
Preferably, the washing lotion of washing residue is the 0.16mol/L salpeter solution.
Preferably, the chloroazotic acid of dissolving ash content is freshly prepared, and promptly 1 volume nitric acid (proportion 1.42) forms with 3 volume hydrochloric acid (proportion 1.18) mixing.
Preferably, to make 5% chloroazotic acid medium (be chloroazotic acid: water=5: 95) to the test solution to be measured of Atomic Absorption Spectrometer.
When implementing the inventive method, analysis result is pressed calibration curve method and is calculated.
Analyzing and testing result calculates:
In the formula:
C represents the concentration (ug/ml) that checks in sample light absorption value corresponding A u on the typical curve;
C
0Represent the concentration (ug/ml) that checks in blank light absorption value corresponding A u on the typical curve;
V represents the volume (ml) of test solution to be measured;
M represents the quality (g) of sample.
Advantage of the present invention is, and is simple and easy to do to the assay method of gold element in the smelting material, and flow process is short, invest little, analysis result accuracy height, favorable reproducibility.
Description of drawings
Fig. 1 is the canonical plotting of the present invention with atomic absorption spectrometry.
Embodiment
Be described in further detail below in conjunction with the analyzing detecting method of drawings and Examples gold element of the present invention.
Embodiment: the analyzing and testing of gold element in the lead anode slurry
The drawing standard curve
Get goldc grains (Au 〉=99.99%) and add aqua regia dissolution, be mixed with the standard solution that contains golden 10ug/ml, make standard series by method step of the present invention and measure and the drawing standard curve.Specific operation process is: pipette 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.50ml, 10.00ml goldstandard solution (1ml=10ug) add the 5ml chloroazotic acid in a series of 50ml volumetric flasks, and the water constant volume shakes up.With atomic absorption spectrometry standard series light absorption value, be horizontal ordinate with the normal concentration, light absorption value is an ordinate, the drawing standard curve.
Sample determination (sample 30-4)
Take by weighing 10.00 gram lead anode slurry samples in the 400ml beaker, add 2 gram tartrate, 200ml nitric acid (4mol/L), heating for dissolving is complete.After treating the test solution cooling, use quick filter paper filtering.Wash beaker, residue each 5～6 times with salpeter solution (0.16mol/L), wash with water 2 times.
Filter paper, residue are put into the 50ml porcelain crucible, place in 750 ℃ of muffle furnaces ashing to take out crucible fully, treat porcelain crucible cooling fully after, add the freshly prepared chloroazotic acid of 15ml, in low temperature place heating for dissolving 10 minutes, treat the solution cooling after, constant volume 200ml shakes up, and is prepared into test solution to be measured.
Get above-mentioned test solution to be measured, select combustion to help than 5:1, slit 0.2mm, lamp current 2mA, negative high voltage 300V is with atomic absorption spectrometry gold element light absorption value.According to the light absorption value of test solution, look into the aforesaid standards working curve, Calculation results: a plurality of analyzing and testing results' of sample lead anode slurry mean value is 23.9 gram/tons, standard deviation 1.05, relative standard deviation 4.65%.
This analysis detection method is suitable for smelting materials such as lead anode slurry, lead bismuth alloy, high silver-colored slag, lead bullion, thick bismuth, thick silver, blister copper.
Claims (9)
1. the analyzing detecting method of gold element in the smelting material comprises the steps:
(1) will add nitric acid and tartrate in the smelting material sample, and carry out heating pretreatment;
(2) after the preprocessing solution cooling, use filter paper filtering, all be transferred on the filter paper residue and washing, make gold element and matrix bismuth, lead, silver and other separation of foreign elements;
(3) filter paper and the residue after will washing put into porcelain crucible, places in the muffle furnace ashing complete;
(4) use the aqua regia dissolution ash content, be prepared into test solution to be measured;
(5) select combustion to help than 5:1, slit 0.2mm, lamp current 2mA, negative high voltage 300V is with atomic absorption spectrometry gold element light absorption value, Calculation results.
2. analyzing detecting method according to claim 1 is characterized in that, during the heating pretreatment sample, the concentration of nitric acid is 4mol/L, and tartrate is solid.
3. analyzing detecting method according to claim 1 is characterized in that, the cleansing solution that the washing residue is used is the salpeter solution of 0.16mol/L.
4. analyzing detecting method according to claim 1 is characterized in that analysis result calculates according to following formula by calibration curve method:
In the formula:
C represents the concentration (ug/ml) that checks in sample light absorption value corresponding A u on the typical curve;
C
0Represent the concentration (ug/ml) that checks in blank light absorption value corresponding A u on the typical curve;
V represents the volume (ml) of test solution to be measured;
M represents the quality (g) of sample.
5. analyzing detecting method according to claim 1 is characterized in that, the chloroazotic acid used of dissolving ash content is that the nitric acid of 1 volume of 1.42 and proportion are that the hydrochloric acid mixing of 3 volumes of 1.18 forms by proportion.
6. analyzing detecting method according to claim 1 is characterized in that, utilizes the light absorption value of atomic absorption spectrometry gold element in the medium of chloroazotic acid: water=5:95.
7. analyzing detecting method according to claim 1 is characterized in that, filter paper and residue are put into porcelain crucible and placed 750 ℃ of muffle furnace ashing complete.
8. analyzing detecting method according to claim 4, it is characterized in that, the plot step of typical curve is: the goldc grains of getting an amount of purity 〉=99.99% adds aqua regia dissolution, be mixed with the standard solution that contains golden 10ug/ml, pipette 0.00ml, 1.00ml, 3.00ml, 5.00ml, 7.50ml, 10.00ml goldstandard solution in a series of 50ml volumetric flasks, add the 5ml chloroazotic acid, the water constant volume, shake up, with atomic absorption spectrometry standard series light absorption value, with the normal concentration is horizontal ordinate, and light absorption value is an ordinate, the drawing standard curve.
9. analyzing detecting method according to claim 1, it is characterized in that test solution to be measured is prepared according to following steps: take by weighing 10.00 gram smelting material samples in the 400ml beaker, add 2 gram tartrate, 200ml concentration is the nitric acid of 4mol/L, and heating for dissolving is complete; After treating the test solution cooling, use quick filter paper filtering; With concentration is salpeter solution washing beaker, the residue each 5～6 times of 0.16mol/L, washes with water 2 times; Filter paper, residue are put into the 50ml porcelain crucible, place in 750 ℃ of muffle furnaces ashing to take out crucible fully, treat porcelain crucible cooling fully after, add the freshly prepared chloroazotic acid of 15ml, heating for dissolving 10 minutes, treat the solution cooling after, constant volume 200ml shakes up.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310178916.1A CN103267736B (en) | 2008-12-18 | 2008-12-18 | The analyzing detecting method of gold element in smelting material |
| CNA2008102401152A CN101424635A (en) | 2008-12-18 | 2008-12-18 | Aurum element analyzing and detecting method in smelting material |
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| CNA2008102401152A CN101424635A (en) | 2008-12-18 | 2008-12-18 | Aurum element analyzing and detecting method in smelting material |
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| CN201310178916.1A Division CN103267736B (en) | 2008-12-18 | 2008-12-18 | The analyzing detecting method of gold element in smelting material |
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| CN201310178916.1A Expired - Fee Related CN103267736B (en) | 2008-12-18 | 2008-12-18 | The analyzing detecting method of gold element in smelting material |
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Cited By (7)
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| GB2488433A (en) * | 2011-02-24 | 2012-08-29 | Denso Corp | Absorbent and method of collecting precious metals |
| CN102866042A (en) * | 2011-07-05 | 2013-01-09 | 内蒙古蒙牛乳业（集团）股份有限公司 | Pretreatment method of Acesulfame-K and detection method for potassium in Acesulfame-K |
| CN103018191A (en) * | 2012-12-04 | 2013-04-03 | 广州有色金属研究院 | Analytic method of trace gold contained in composition brass |
| CN103954524A (en) * | 2013-12-11 | 2014-07-30 | 西部矿业股份有限公司 | Simple and rapid method for accurate determination of silver in lead anode mud |
| CN104089798A (en) * | 2013-11-21 | 2014-10-08 | 云南黄金矿业集团股份有限公司 | Gold content determination method |
| CN107036988A (en) * | 2017-05-18 | 2017-08-11 | 山东玉皇新能源科技有限公司 | It is a kind of to detect the method that graphene Gold Samples belong to constituent content |
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| CN107014766A (en) * | 2017-06-02 | 2017-08-04 | 江苏理工学院 | Gold, Palladium deter-mination method in a kind of decopper(ing) slag of copper anode mud wet processing process |
| CN107238578A (en) * | 2017-06-02 | 2017-10-10 | 江苏理工学院 | A kind of silver determination method in decopper(ing) slag of copper anode mud wet processing process |
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-
2008
- 2008-12-18 CN CNA2008102401152A patent/CN101424635A/en active Pending
- 2008-12-18 CN CN201310178916.1A patent/CN103267736B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2488433A (en) * | 2011-02-24 | 2012-08-29 | Denso Corp | Absorbent and method of collecting precious metals |
| US8535625B2 (en) | 2011-02-24 | 2013-09-17 | Denso Corporation | Adsorbent and method of collecting precious metal using the same |
| GB2488433B (en) * | 2011-02-24 | 2017-08-16 | Denso Corp | Carbohydrate adsorbent and method of collecting precious metals |
| CN102866042A (en) * | 2011-07-05 | 2013-01-09 | 内蒙古蒙牛乳业（集团）股份有限公司 | Pretreatment method of Acesulfame-K and detection method for potassium in Acesulfame-K |
| CN102866042B (en) * | 2011-07-05 | 2014-09-10 | 内蒙古蒙牛乳业（集团）股份有限公司 | Pretreatment method of Acesulfame-K and detection method for potassium in Acesulfame-K |
| CN103018191A (en) * | 2012-12-04 | 2013-04-03 | 广州有色金属研究院 | Analytic method of trace gold contained in composition brass |
| CN104089798A (en) * | 2013-11-21 | 2014-10-08 | 云南黄金矿业集团股份有限公司 | Gold content determination method |
| CN103954524A (en) * | 2013-12-11 | 2014-07-30 | 西部矿业股份有限公司 | Simple and rapid method for accurate determination of silver in lead anode mud |
| CN103954524B (en) * | 2013-12-11 | 2017-02-15 | 西部矿业股份有限公司 | Simple and rapid method for accurate determination of silver in lead anode mud |
| CN107036988A (en) * | 2017-05-18 | 2017-08-11 | 山东玉皇新能源科技有限公司 | It is a kind of to detect the method that graphene Gold Samples belong to constituent content |
| CN107991207A (en) * | 2017-11-29 | 2018-05-04 | 长春黄金研究院 | Golden assay method in a kind of high impurity copper anode mud |
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| CN103267736A (en) | 2013-08-28 |
| CN103267736B (en) | 2015-09-09 |
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Application publication date: 20090506 |