CN103575668A - Method for measuring gold content in carbon-containing ore by using spectrophotometry - Google Patents
Method for measuring gold content in carbon-containing ore by using spectrophotometry Download PDFInfo
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- CN103575668A CN103575668A CN201210272656.XA CN201210272656A CN103575668A CN 103575668 A CN103575668 A CN 103575668A CN 201210272656 A CN201210272656 A CN 201210272656A CN 103575668 A CN103575668 A CN 103575668A
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Abstract
The invention discloses a method for measuring the gold content in carbon-containing ore by using spectrophotometry. The method comprises the following steps: weighing an ore sample in a beaker, and wetting by using a small amount of water; adding concentrated H2SO4, heating the concentrated H2SO4 on an electric heating plate until the concentrated H2SO4 is nearly dry, adding concentrated HNO3 for treatment, heating until nitrogen-free oxide smoke is generated, adding the concentrated HNO3 again, adding KClO3 in batches, and heating until black residues and sulfur agglomerations are generated; adding aqua regia for complete decomposition, and cooling; pouring the solution into a microfiltration membrane filter, performing suction filtration by using a vacuum pump, taking down a separation enrichment column after the filtering is finished, arranging the separation enrichment column on a colorimetric tube, adding eluent into the separation enrichment column for washing gold, respectively adding a hot lauryl sodium sulfate solution, a mask-buffer solution and a thiomicoler's ketone solution, diluting by using water, uniformly shaking, and standing for 3-5 minutes; and measuring absorbancy according to sample analysis, thus obtaining the weight of gold in each ton of samples. The method is rapid and accurate to measure and simple and convenient to operate.
Description
Technical field
The present invention relates to a kind of method with spectrophotometry carbon containing Gold in Ores content.
Background technology
During geology both domestic and external, ,Jin smeltery, mine are all widely used in fire assaying as the most reliable analytical approach producing.Due to fire assaying, to have cost high, and operating process is complicated, and labour intensity is large, need analyst experienced, skilled operation could be competent at this work, if operation does not pass a test, cannot Accurate Determining, furthermore the weak point such as analytic sample in enormous quantities.Along with scientific and technical development, analyze golden new technology more and more, analytical instrument is also more and more advanced, fire assaying and other method comparison, its running program is grown and is needed certain skill, has many analytical work persons to attempt to replace fire assaying by other analytical approach.
At present to golden analysis except fire assaying, adopt spectrophotometry seldom, and company laboratory is to Gold in Ores, analysis has adopted spectrophotometry to apply more than 10 year, analysis result is through contrasting with fire assaying, its result is substantially consistent, and analysis to carbon containing Gold in Ores, the dissolving method that employing company laboratory is current, can't resolve problem, easily cause analysis result obviously on the low side, give ground, adopt, choosing, smelting is produced and is brought misleading, so its dissolving method is restricted, spectrophotometric method to carbon containing Gold in Ores analysis cannot apply.
Summary of the invention
This technical matters that will solve is to provide a kind of mensuration quick and precisely, simple to operation, the method with spectrophotometry carbon containing Gold in Ores content with low cost.
For solving this technical problem, the technical solution used in the present invention is:
A method with spectrophotometry carbon containing Gold in Ores content, the steps include: to take a certain amount of sample ore in beaker, with the wetting sample ore of little water; Add dense H
2sO
4, on electric hot plate, be heated near doing, then add dense HNO
3process, be heated to, after nitrogenfree oxide cigarette, again add dense HNO
3, and gradation adds a certain amount of KClO
3, be heated to without black residue and sulphur caking; Add chloroazotic acid to decompose completely, cooling; Solution is poured in nuclepore membrane filter, use vacuum pump suction filtration, after filtration, take off separation and concentration pillar, be placed on color comparison tube, add eluent to abacus in separation and concentration pillar, add respectively hot sodium dodecyl sulfate solution, add to shelter-buffer solution, add thiomicoler's ketone solution, dilute with water, shake up, place 3～5 minutes; Use 1cm cuvette, take reagent blank as reference, use spectrophotometry absorbance; Analyze per sample the absorbance recording, from goldstandard curve, find the micrograms of corresponding gold, with checking in golden micrograms divided by the grams that claims sample weight, just can obtain in sample per ton containing golden grams.
The described sample ore taking is 10.0g.
Describedly add dense H
2sO
4amount be 5ml, described in add dense HNO
3amount be that 20ml processes 2-3 time, describedly again add dense HNO
3amount be 20ml.
The described KClO that adds
3number of times be 2 times, each each 1 gram.
The volume of described color comparison tube is 50ml, it is described that to add the amount of eluent be 16ml, described in to add the amount of hot sodium dodecyl sulfate solution be 3.0ml, described in to add the amount of shelter-buffer solution be 2.0ml, it is described that to add the amount of thiomicoler's ketone solution be 2.0ml, described in be diluted with water to 25ml.
At wavelength 548nm place, measure absorbance.
The instrument that described spectrophotometric method is used is 721 type spectrophotometric method meters.
The invention has the beneficial effects as follows: analyze accurately fast, simple to operation, and analysis cost is only 1/5 of assaying of firing method method analysis cost, analytical cycle only has 1/3 of assaying of firing method method; Expanded the usable range of spectrophotometric method.
Embodiment
Take 10.0g sample ore in 400mL beaker, with the wetting sample ore of little water, add the dense H of 5mL
2sO
4, on electric hot plate, be heated near doing, then add the dense HNO of 20mL
3process 2～3 times (carefully spilling) and be heated to after nitrogenfree oxide cigarette, add the dense HNO of 20mL
3, gradation adds a certain amount of KClO
3be heated to without black residue and sulphur caking, add again chloroazotic acid to decompose completely, after cooling, solution is poured in nuclepore membrane filter, used vacuum pump suction filtration, after filtration, take off separation and concentration pillar, be placed on 50mL color comparison tube, add 16mL eluent to abacus in separation and concentration pillar, add respectively the sodium dodecyl sulfate solution of 3.0mL heat, add shelter-buffer solution of 2.0mL, 2.0mLTMK solution, be diluted with water to 25mL, shake up, place 3～5min, use 1cm cuvette, take reagent blank as reference, at wavelength 548nm place, measure absorbance.
The contrast of analysis result:
The contrast of spectrophotometry result and fire assaying
The method is through practical application, company laboratory adopts spectrophotometric analysis to carbon containing sample now, analysis result is satisfied, the successful Application of the method had thoroughly replaced in the past and only to adopt fire assaying to measure to the analysis of carbon containing Gold in Ores, expanded the usable range of spectrophotometric method, analyze accurately fast, and analysis cost is only 1/5 of assaying of firing method method analysis cost, analytical cycle only has 1/3 of assaying of firing method method; Unrestricted to sample number, can guarantee to accomplish that sample is analyzed at any time at any time, thereby strengthen the directive function to producing, reduced analyst's labour intensity, improved analyst's operating environment.
Gold mine sample for carbon containing, sulphur; The method is worthy of promotion and application, and prospect is very wide.
Main agents:
It is pure that sulfuric acid, hydrochloric acid, nitric acid, potash chlorate are analysis.
Eluent: adding distil water 200mL in the brown reagent bottle of 500mL, then add 4.0g anhydrous sodium sulfate, and 1.0g potassium iodide and 0.2g ascorbic acid, 3.0mL (volume ratio is 1:1) ammoniacal liquor, then add 200mL distilled water, shake reagent is dissolved completely.Room temperature is lower than 25
0during C, its term of validity 48h.
Sodium dodecyl sulfate solution (SDS solution): claim 10g lauryl sodium sulfate in 400mL beaker, add 200mL distilled water, add thermal agitation and make reagent dissolve (do not boil, otherwise solution easily overflowing outside cup) completely, use miillpore filter suction filtration, obtain the solution of clarification.
Masking buffer liquid: PH=3.5～3.8; In 1000mL beaker, add 400mL water and 17.5gEDTA disodium, after heating for dissolving, add again 84g citric acid and 84mL glacial acetic acid, and add 100mL water (now having white precipitate disengages), under constantly stirring with glass bar, and add strong aqua adjusting.
Thiomicoler's ketone solution (being called for short TMK solution): claim 50mgTMK in the 100mL graduated cylinder of drying, add a small amount of acetone, shake 3～4min, impel reagent fully to dissolve.With absolute ethyl alcohol, be diluted to 100mL, standing a moment, then use dry glass funnel (filling in a small amount of absorbent cotton in filler neck) to filter.Then add respectively 100mL and 50mL absolute ethyl alcohol in graduated cylinder, in standing a moment, with funnel, filter, whole filtrate is collected in a Brown Glass Brown glass bottles and jars only and (with on black paper bag, keeps in Dark Place, generally use and be advisable for 1～2 week), cover Bo Sai, shake up.
Wang aqueous solution: by hydrochloric acid and nitric acid volume ratio, be 3:1 preparation chloroazotic acid, matching while using.
Claims (7)
1. by a method for spectrophotometry carbon containing Gold in Ores content, the steps include:
(1) take a certain amount of sample ore in beaker, with the wetting sample ore of little water;
(2) add dense H
2sO
4, on electric hot plate, be heated near doing, then add dense HNO
3process, be heated to, after nitrogenfree oxide cigarette, again add dense HNO
3, and gradation adds a certain amount of KClO
3, be heated to without black residue and sulphur caking;
(3) add chloroazotic acid to decompose completely, cooling;
(4) solution is poured in nuclepore membrane filter, use vacuum pump suction filtration, after filtration, take off separation and concentration pillar, be placed on color comparison tube, add eluent to abacus in separation and concentration pillar, add respectively hot sodium dodecyl sulfate solution, add to shelter-buffer solution, add thiomicoler's ketone solution, dilute with water, shake up, place 3～5 minutes;
(5) use 1cm cuvette, take reagent blank as reference, use spectrophotometry absorbance;
(6) analyze per sample the absorbance recording, from goldstandard curve, find the micrograms of corresponding gold, with checking in golden micrograms divided by the grams that claims sample weight, just can obtain in sample per ton containing golden grams.
2. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, is characterized in that: described in the sample ore that takes be 10.0g.
3. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, is characterized in that: described in add dense H
2sO
4amount be 5ml, described in add dense HNO
3amount be that 20ml processes 2-3 time, describedly again add dense HNO
3amount be 20ml.
4. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, is characterized in that: described in add KClO
3number of times be 2 times, each each 1 gram.
5. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, it is characterized in that: the volume of described color comparison tube is 50ml, it is described that to add the amount of eluent be 16ml, it is described that to add the amount of hot sodium dodecyl sulfate solution be 3.0ml, it is described that to add the amount of shelter-buffer solution be 2.0ml, it is described that to add the amount of thiomicoler's ketone solution be 2.0ml, described in be diluted with water to 25ml.
6. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, is characterized in that: at wavelength 548nm place, measure absorbance.
7. the method with spectrophotometry carbon containing Gold in Ores content according to claim 1, is characterized in that: the instrument that described spectrophotometric method is used is 721 type spectrophotometric method meters.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596544A (en) * | 2017-02-07 | 2017-04-26 | 班俊生 | Field rapid determination method for gold content of gold ore |
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| CA1279205C (en) * | 1986-12-29 | 1991-01-22 | Roland W. Hatch | Process for the determination of gold in rocks and ores, and apparatustherefor |
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| CN102323250A (en) * | 2011-06-15 | 2012-01-18 | 金川集团有限公司 | Method for quickly determining gold, palladium, platinum, rhodium, iridium, silver, nickel, copper and iron in rare and precious metal system |
| CN102331361A (en) * | 2011-08-25 | 2012-01-25 | 广西地博矿业集团股份有限公司 | Pretreatment method for testing micro-granular gold ore containing organic carbon through atomic absorption spectrometry |
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2012
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|---|---|---|---|---|
| CA1279205C (en) * | 1986-12-29 | 1991-01-22 | Roland W. Hatch | Process for the determination of gold in rocks and ores, and apparatustherefor |
| CN101046453A (en) * | 2007-04-24 | 2007-10-03 | 青海西部矿业科技有限公司 | Iodometry process of measuring gold content in high accuracy and precision |
| CN201382901Y (en) * | 2009-03-04 | 2010-01-13 | 吉林大学 | Portable trace gold quick analyzer |
| CN102323250A (en) * | 2011-06-15 | 2012-01-18 | 金川集团有限公司 | Method for quickly determining gold, palladium, platinum, rhodium, iridium, silver, nickel, copper and iron in rare and precious metal system |
| CN102331361A (en) * | 2011-08-25 | 2012-01-25 | 广西地博矿业集团股份有限公司 | Pretreatment method for testing micro-granular gold ore containing organic carbon through atomic absorption spectrometry |
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| 符永际: "分光光度法测定化探样品中的金", 《黄金》, vol. 31, no. 7, 31 December 2010 (2010-12-31), pages 56 - 57 * |
| 符永际: "含碳矿石中金的分析测定", 《黄金科学技术》, vol. 16, no. 16, 31 December 2008 (2008-12-31), pages 42 - 43 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106596544A (en) * | 2017-02-07 | 2017-04-26 | 班俊生 | Field rapid determination method for gold content of gold ore |
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Application publication date: 20140212 |