CN107703121A - The assay method of rhenium content in rehenic acid ammonium - Google Patents

The assay method of rhenium content in rehenic acid ammonium Download PDF

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CN107703121A
CN107703121A CN201710976672.XA CN201710976672A CN107703121A CN 107703121 A CN107703121 A CN 107703121A CN 201710976672 A CN201710976672 A CN 201710976672A CN 107703121 A CN107703121 A CN 107703121A
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rhenium
platinum
electrolysis
acid ammonium
assay method
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钱庆长
吴德珍
史静
倪莹
江玲玲
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Jinguan Copper Industry Branch of Tongling Nonferrous Metals Group Holding Co Ltd
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Jinguan Copper Industry Branch of Tongling Nonferrous Metals Group Holding Co Ltd
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    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The present invention relates to chemical analysis technology field, and in particular to the assay method of rhenium content in a kind of rehenic acid ammonium;By using platinum electrode as anodic-cathodic, being electrolysed under certain density electrolyte and certain current density, electrolyte is stirred using bubble caused by platinum anode, whole electrolytic process is not turned on stirring and heater, makes high rhenium acid group ion (ReO4 ) be reduced to rhenium metal (Re) and be deposited in the platinum negative electrode of known quality, through drying, weigh, produce the quality of the rhenium deposited in platinum cathode;The Determination of Trace Rhenium being electrolysed in Liquid Residue is subjected to correction measure with ICP AES methods simultaneously;The present invention uses electrolysis and ICP AES methods simultaneously, ensure that the accuracy of measurement result.

Description

The assay method of rhenium content in rehenic acid ammonium
Technical field
The present invention relates to chemical analysis technology field, and in particular to the assay method of rhenium content in a kind of rehenic acid ammonium.
Background technology
Rhenium is a kind of yttrium, and its content in the earth's crust is extremely low, be only distributed on a small quantity molybdenite, Rare Earth Mine and In Nb-Ta mineral.Rhenium metal has dystectic characteristic, is commonly used for refining the catalyst of oil, and in high temperature alloy, electron tube knot There is wide application in the fields such as structure material, Aero-Space specific alloy, environmental protection.At present, it is best to prepare simple metal rhenium Method is with its industrial compound rehenic acid ammonium of hydrogen reducing.Usually contain certain impurity in the rehenic acid ammonium industrially generated, its The species and content of impurity have a strong impact on the purity of sample, and the height for detecting rhenium content in rehenic acid ammonium is the weight of judgement sample purity Want index.At present, although using the rhenium content in photometry measure tungsten-rhenium alloy, and ICP-AES method (inductance couplings are used Close plasma atomic emission spectrometry) rhenium in measure uranium ore, but either rhenium alloys or rhenium ore, rhenium therein contain Amount is all extremely low, and rhenium content is higher by comparison, in rehenic acid ammonium, there is nearly 70%.Influenceed by luminosity transmission, using photometry or When ICP-AES methods determine the rhenium content in rehenic acid ammonium, deviation is larger between its measurement result and actual value, and reappearance is also bad, In other words, the measure of high content rhenium rehenic acid ammonium is not particularly suited for suitable for determining the method for low content rhenium.
For the measure of high content rhenium in rehenic acid ammonium, in the prior art, there are ICP-AES methods and tetraphenylarsonium chloride hydrochloride precipitation Two kinds of gravimetric method.ICP-AES methods need first to determine the impurity content in rehenic acid ammonium, then deduct impurity content from entirety to retrodict The rhenium content gone out in rehenic acid ammonium.Missed because the measurement result of single impurity content and the cumulative of multiple impurity measurement results are present Difference, therefore the problem of measurement result inaccuracy be present in the method, and needed in continuous mode by evaporating repeatedly by rhenium with sulfuration rhenium Form remove, evaporation time length, energy resource consumption is big.And detection time be present using tetraphenylarsonium chloride hydrochloride Sediment weight rule The defects of Chang ﹑ poor anti jamming capabilities.
The content of the invention
It is an object of the invention to provide rhenium in the rehenic acid ammonium that a kind of method is simple and environmentally-friendly, accuracy is high, detection speed is fast The assay method of content.
To achieve the above object, the technical solution adopted by the present invention is:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) it is m by quality0Rehenic acid ammonium be dissolved in water, sulfuric acid and ammonium sulfate are added into Ammonium rhenate solution, is made into electrolysis Liquid;
(2) platinum electrode is pre-processed, obtains platinum anode and platinum cathode;
(3) take out platinum cathode to be dried, cool down, first time accurate weighing platinum cathode quality;
(4) platinum anode and platinum cathode are immersed in electrolyte, at room temperature, be powered electrolysis;
(5) after electrolysis completely, take out platinum cathode and be dried, cool down, second of accurate weighing platinum cathode quality;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality m of the rhenium of extremely upper deposition1
(7) with the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods, rhenium in electrolysis Liquid Residue is calculated Quality m2
(8) mass fraction of rhenium is calculated according to formula (a):
W(Re)=(m1+m2)/m0× 100% ... ... ... ... (a)
In formula:
W(Re)The mass fraction of rhenium, numerical value are represented with % in-rehenic acid ammonium;
m0、m1、m2, unit is gram (g).
Beneficial effect is caused by above-mentioned technical proposal:
Using platinum electrode as anodic-cathodic, it is electrolysed, is utilized under certain density electrolyte and certain current density Bubble caused by platinum anode stirs electrolyte, and whole electrolytic process is not turned on stirring and heater, make high rhenium acid group ion (ReO4 -) be reduced to rhenium metal (Re) and be deposited in the platinum negative electrode of known quality, through drying, weigh, produce and deposited in platinum cathode Rhenium quality.The Determination of Trace Rhenium being electrolysed in Liquid Residue is subjected to correction measure with ICP-AES methods simultaneously.Due in electrode Liquid Residue The content range of rhenium is in ICP-AES detection range, so can be entered using ICP-AES methods to the content of rhenium in electrode Liquid Residue Row Accurate Determining.According on electrode it is increased and merge correction rhenium quality, just can accurately determine rhenium in rehenic acid ammonium Content.The present invention uses electrolysis and ICP-AES methods simultaneously, ensure that the accuracy of measurement result.Method provided by the invention It is simple and convenient, green, detection speed is fast.
More specifically scheme is:The concentration of rehenic acid ammonium is 3.5-4.5g/L in the electrolyte of the step (1), sulfuric acid it is dense Spend for 3-8g/L, the concentration of ammonium sulfate is 15-25g/L.If sulfuric acid concentration is higher, electrolyte display color is then partially deep, solution In coloring matter easily absorption beaker inwall influence observe, while can cause be electrolysed Liquid Residue in rhenium content it is higher.
Preferably, the preprocess method in the step (2) is:Platinum electrode is placed in 50vt% nitric acid and boils 4- 5min, the impurity being attached on platinum electrode is removed, taking-up is rinsed well with water, 1-2min is then boiled in boiling water, with thorough The nitric acid of platinum electrode surface is removed, taking-up is embathed with absolute ethyl alcohol to be produced twice.
Preferably, the drying temperature in the step (2) and step (5) is 100-110 DEG C.
Specifically, the electrolytic method in the step (4) is:First electrolyte is poured into beaker, then by platinum anode and Platinum cathode is arranged on electrolysis apparatus, makes platinum guaze submergence in the electrolytic solution, burning is covered with the polytetrafluoroethylene (PTFE) ware or glass dish splitted Cup, changes the concentration of electrolyte to prevent moisture evaporation, while prevents the foreign matter in air from entering in electrolyte.Adjusting electric current is 3.5-4.5A, current potential 368mv, start to be electrolysed, it is complete to being electrolysed.Electric current can not be too high in electrolytic process, otherwise can cause platinum Rhenium deposition velocity is too fast on electrode forms spongy deposit and comes off, and the rhenium deposit coating obtained on electrode is not fine and close not Uniformly, so influence testing result reappearance;Electric current is too low, and the rhenium deposit coating obtained on electrode is uniform firm, but It is time-consuming long, influence the ageing of detection.
To ensure the accuracy of measurement result, before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass is washed with deionized Ware inner surface, wall of cup and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on without rhenium separate out, that is, represent be electrolysed Entirely.
To ensure the rhenium content range in electrolysis Liquid Residue in ICP-AES detection range, the electricity in the step (4) The solution time is 4-6 hours.
To be further ensured that the accuracy of measurement result, in the step (5) after electrolysis completely, do not cut off the electricity supply first, Platinum cathode is eluted by several times with deionized water, power supply is then turned off, is embathed twice with absolute ethyl alcohol, then be dried, weigh.
Specifically, the wavelength that uses of ICP-AES methods is 197.313nm in the step (7).
Embodiment
1-5 is further described to technical scheme disclosed by the invention with reference to embodiments:
Embodiment 1:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) 0.9997g rehenic acid ammoniums are weighed to be dissolved in 150ml water, then add the sulfuric acid solution that 50.0ml concentration is 25g/L With 5g ammonium sulfate, after dissolving completely, 250ml is diluted to, produces electrolyte;
(2) platinum electrode is placed in 50vt% nitric acid and boils 4min, taking-up is rinsed well with water, is then boiled in boiling water 2min is boiled, taking-up is embathed twice with absolute ethyl alcohol, obtains platinum anode and platinum cathode;
(3) under conditions of 105 DEG C, 4min, cooling, first time accurate weighing platinum cathode quality are dried to platinum cathode 19.1973g;
(4) first electrolyte is poured into beaker, then platinum anode and platinum cathode is arranged on electrolysis apparatus, make platinum guaze or platinum Piece submerges in the electrolytic solution, covers beaker with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, regulation electric current is 4.0A, and current potential is 368mv, start to be electrolysed at room temperature;Before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass dish inner surface, cup is washed with deionized Wall and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on separated out without rhenium, that is, represent that electrolysis is complete;
(5) after electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, takes Go out platinum cathode, embathed twice with absolute ethyl alcohol, then at 105 DEG C, dry 4min, cooling, second of accurate weighing platinum cathode matter Measure 19.8892g;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality 0.6919g of the rhenium of extremely upper deposition;
(7) electrolyte being electrolysed after separating out rhenium is moved into 250ml volumetric flasks, is diluted with water to scale, shakes up, With the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods under 197.313nm wavelength, electrolysis Liquid Residue is calculated The quality 0.0007g of middle rhenium;
(8) the mass fraction X of rhenium is calculated1
W (Re)=(0.6919+0.0007)/0.9997 × 100%=69.28%.
Embodiment 2:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) 1.0040g rehenic acid ammoniums are weighed to be dissolved in 150ml water, then add the sulfuric acid solution that 75.0ml concentration is 25g/L With 5g ammonium sulfate, after dissolving completely, 250ml is diluted to, produces electrolyte;
(2) platinum electrode is placed in 50vt% nitric acid and boils 5min, taking-up is rinsed well with water, is then boiled in boiling water 1min is boiled, taking-up is embathed twice with absolute ethyl alcohol, obtains platinum anode and platinum cathode;
(3) under conditions of 105 DEG C, 3min, cooling, first time accurate weighing platinum cathode quality are dried to platinum cathode 19.1975g;
(4) first electrolyte is poured into beaker, then platinum anode and platinum cathode is arranged on electrolysis apparatus, make platinum guaze or platinum Piece submerges in the electrolytic solution, covers beaker with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, regulation electric current is 4.0A, and current potential is 368mv, start to be electrolysed at room temperature;Before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass dish inner surface, cup is washed with deionized Wall and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on separated out without rhenium, that is, represent that electrolysis is complete;
(5) after electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, takes Go out platinum cathode, embathed twice with absolute ethyl alcohol, then at 105 DEG C, dry 3min, cooling, second of accurate weighing platinum cathode matter Measure 19.8921g;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality 0.6946g of the rhenium of extremely upper deposition;
(7) electrolyte being electrolysed after separating out rhenium is moved into 250ml volumetric flasks, is diluted with water to scale, shakes up, With the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods under 197.313nm wavelength, electrolysis Liquid Residue is calculated The quality 0.0021g of middle rhenium;
(8) the mass fraction X of rhenium is calculated2
W (Re)=(0.6946+0.0021)/1.0040 × 100%=69.39%.
Embodiment 3:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) 1.0007g rehenic acid ammoniums are weighed to be dissolved in 150ml water, then add the sulfuric acid solution that 40.0ml concentration is 25g/L With 5.5g ammonium sulfate, after dissolving completely, 250ml is diluted to, produces electrolyte;
(2) platinum electrode is placed in 50vt% nitric acid and boils 5min, taking-up is rinsed well with water, is then boiled in boiling water 2min is boiled, taking-up is embathed twice with absolute ethyl alcohol, obtains platinum anode and platinum cathode;
(3) under conditions of 105 DEG C, 5min, cooling, first time accurate weighing platinum cathode quality are dried to platinum cathode 19.1973g;
(4) first electrolyte is poured into beaker, then platinum anode and platinum cathode is arranged on electrolysis apparatus, make platinum guaze or platinum Piece submerges in the electrolytic solution, covers beaker with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, regulation electric current is 4.0A, and current potential is 368mv, start to be electrolysed at room temperature;Before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass dish inner surface, cup is washed with deionized Wall and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on separated out without rhenium, that is, represent that electrolysis is complete;
(5) after electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, takes Go out platinum cathode, embathed twice with absolute ethyl alcohol, then at 105 DEG C, dry 5min, cooling, second of accurate weighing platinum cathode matter Measure 19.8871g;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality 0.6898g of the rhenium of extremely upper deposition;
(7) electrolyte being electrolysed after separating out rhenium is moved into 250ml volumetric flasks, is diluted with water to scale, shakes up, With the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods under 197.313nm wavelength, electrolysis Liquid Residue is calculated The quality 0.0027g of middle rhenium;
(8) the mass fraction X of rhenium is calculated3
W (Re)=(0.6898+0.0027)/1.0007 × 100%=69.20%.
Embodiment 4:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) 1.0002g rehenic acid ammoniums are weighed to be dissolved in 150ml water, then add the sulfuric acid solution that 65.0ml concentration is 25g/L With 4.5g ammonium sulfate, after dissolving completely, 250ml is diluted to, produces electrolyte;
(2) platinum electrode is placed in 50vt% nitric acid and boils 4min, taking-up is rinsed well with water, is then boiled in boiling water 1min is boiled, taking-up is embathed twice with absolute ethyl alcohol, obtains platinum anode and platinum cathode;
(3) under conditions of 110 DEG C, 5min, cooling, first time accurate weighing platinum cathode quality are dried to platinum cathode 19.1967g;
(4) first electrolyte is poured into beaker, then platinum anode and platinum cathode is arranged on electrolysis apparatus, make platinum guaze or platinum Piece submerges in the electrolytic solution, covers beaker with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, regulation electric current is 3.5A, and current potential is 368mv, start to be electrolysed at room temperature;Before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass dish inner surface, cup is washed with deionized Wall and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on separated out without rhenium, that is, represent that electrolysis is complete;
(5) after electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, takes Go out platinum cathode, embathed twice with absolute ethyl alcohol, then at 110 DEG C, dry 5min, cooling, second of accurate weighing platinum cathode matter Measure 19.8870g;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality 0.6903g of the rhenium of extremely upper deposition;
(7) electrolyte being electrolysed after separating out rhenium is moved into 250ml volumetric flasks, is diluted with water to scale, shakes up, With the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods under 197.313nm wavelength, electrolysis Liquid Residue is calculated The quality 0.0034g of middle rhenium;
(8) the mass fraction X of rhenium is calculated4
W (Re)=(0.6903+0.0034)/1.0002 × 100%=69.36%.
Embodiment 5:
The assay method of rhenium content, comprises the following steps in a kind of rehenic acid ammonium:
(1) 1.0018g rehenic acid ammoniums are weighed to be dissolved in 150ml water, then add the sulfuric acid solution that 50.0ml concentration is 25g/L With 6g ammonium sulfate, after dissolving completely, 250ml is diluted to, produces electrolyte;
(2) platinum electrode is placed in 50vt% nitric acid and boils 4min, taking-up is rinsed well with water, is then boiled in boiling water 1min is boiled, taking-up is embathed twice with absolute ethyl alcohol, obtains platinum anode and platinum cathode;
(3) under conditions of 100 DEG C, 5min, cooling, first time accurate weighing platinum cathode quality are dried to platinum cathode 19.1971g;
(4) first electrolyte is poured into beaker, then platinum anode and platinum cathode is arranged on electrolysis apparatus, make platinum guaze or platinum Piece submerges in the electrolytic solution, covers beaker with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, regulation electric current is 4.0A, and current potential is 368mv, start to be electrolysed at room temperature;Before electrolysis terminates, polytetrafluoroethylene (PTFE) ware or glass dish inner surface, cup is washed with deionized Wall and electrode stem, continue electrolysis 30 minutes, to the platinum cathode newly submerged on separated out without rhenium, that is, represent that electrolysis is complete;
(5) after electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, takes Go out platinum cathode, embathed twice with absolute ethyl alcohol, then at 100 DEG C, dry 5min, cooling, second of accurate weighing platinum cathode matter Measure 19.8905g;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, it is cloudy to obtain platinum The quality 0.6934g of the rhenium of extremely upper deposition;
(7) electrolyte being electrolysed after separating out rhenium is moved into 250ml volumetric flasks, is diluted with water to scale, shakes up, With the concentration of rhenium in the electrolysis Liquid Residue after the measurement electrolysis completely of ICP-AES methods under 197.313nm wavelength, electrolysis Liquid Residue is calculated The quality 0.0008g of middle rhenium;
(8) the mass fraction X of rhenium is calculated5
W (Re)=(0.6934+0.0008)/1.0018 × 100%=69.30%.
The relative standard deviation and rate of recovery difference of the mass fraction of calculating rhenium are as shown in Table 1 and Table 2:
The W of table 1 (Re) relative standard deviation (n=5)
The Rhenium recovery rate of table 2
Above-mentioned result of calculation shows:The Rhenium recovery rate obtained by method provided by the invention between 99%~102%, Relative standard deviation is less than 0.11%.As can be seen here, method favorable reproducibility provided by the invention, can rhenium in Accurate Determining rehenic acid ammonium Content.In fact, the minute of this method is no more than 8 hours, for prior art, has and take short, detection speed Fast advantage.

Claims (9)

1. the assay method of rhenium content in a kind of rehenic acid ammonium, it is characterised in that comprise the following steps:
(1) it is m by quality0Rehenic acid ammonium be dissolved in water, sulfuric acid and ammonium sulfate are added into Ammonium rhenate solution, is made into electrolyte;
(2) platinum electrode is pre-processed, obtains platinum anode and platinum cathode;
(3) take out platinum cathode to be dried, cool down, first time accurate weighing platinum cathode quality;
(4) platinum anode and platinum cathode are immersed in electrolyte, at room temperature, be powered electrolysis;
(5) after electrolysis completely, take out platinum cathode and be dried, cool down, second of accurate weighing platinum cathode quality;
(6) the of poor quality of platinum cathode and the platinum cathode of first time accurate weighing of second of accurate weighing is calculated, is obtained in platinum cathode The quality m of the rhenium of deposition1
(7) concentration for being electrolysed rhenium in Liquid Residue with the measurement electrolysis of ICP-AES methods after complete, the matter of rhenium in electrolysis Liquid Residue is calculated Measure m2
(8) mass fraction of rhenium is calculated according to formula (a):
W(Re)=(m1+m2)/m0× 100% ... ... ... ... (a)
In formula:
W(Re)The mass fraction of rhenium, numerical value are represented with % in-rehenic acid ammonium;
m0、m1、m2, unit is gram (g).
2. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that the electricity of the step (1) The concentration for solving rehenic acid ammonium in liquid is 3.5-4.5g/L, and the concentration of sulfuric acid is 3-8g/L, and the concentration of ammonium sulfate is 15-25g/L.
3. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that in the step (2) Preprocess method is:Platinum electrode is placed in 50vt% nitric acid and boils 4-5min, taking-up is rinsed well with water, then in boiling water In boil 1-2min, taking-up is embathed with absolute ethyl alcohol to be produced twice.
4. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that the step (2) and step Suddenly the drying temperature in (5) is 100-110 DEG C.
5. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that in the step (4) Electrolytic method is:First electrolyte is poured into beaker, then platinum anode and platinum cathode are arranged on electrolysis apparatus, make platinum guaze or platinum Piece is submerged in the electrolytic solution, and beaker is covered with the polytetrafluoroethylene (PTFE) ware or glass dish splitted, adjusts electric current between 3.5-4.5A, Current potential is 368mv, starts to be electrolysed, complete to being electrolysed.
6. the assay method of rhenium content in rehenic acid ammonium according to claim 5, it is characterised in that before electrolysis terminates, use Deionized water washs polytetrafluoroethylene (PTFE) ware or glass dish inner surface, wall of cup and electrode stem, continues electrolysis 30 minutes, to what is newly submerged Separated out in platinum cathode without rhenium, that is, represent that electrolysis is complete.
7. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that in the step (4) Electrolysis time is 4-6 hours.
8. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that in the step (5) After electrolysis completely, do not cut off the electricity supply first, platinum cathode is eluted by several times with deionized water, power supply is then turned off, is soaked with absolute ethyl alcohol Wash twice, then be dried, weigh.
9. the assay method of rhenium content in rehenic acid ammonium according to claim 1, it is characterised in that in the step (7) ICP-AES methods are 197.313nm using wavelength.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161929A (en) * 2018-09-13 2019-01-08 浙江工业大学 A kind of method of electrodeposit metals rhenium

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101303286A (en) * 2008-07-02 2008-11-12 新疆新鑫矿业股份有限公司 Method for rapidly measuring copper content
CN104897505A (en) * 2015-06-01 2015-09-09 贵州天义电器有限责任公司 Method for analyzing copper content in red copper by using electrolytic process and atomic absorption spectroscopy together
CN106430320A (en) * 2016-09-19 2017-02-22 西北有色金属研究院 Method for recycling rhenium from tungsten-rhenium alloy waste

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101303286A (en) * 2008-07-02 2008-11-12 新疆新鑫矿业股份有限公司 Method for rapidly measuring copper content
CN104897505A (en) * 2015-06-01 2015-09-09 贵州天义电器有限责任公司 Method for analyzing copper content in red copper by using electrolytic process and atomic absorption spectroscopy together
CN106430320A (en) * 2016-09-19 2017-02-22 西北有色金属研究院 Method for recycling rhenium from tungsten-rhenium alloy waste

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
王明伟: "《模具材料及表面强化技术》", 31 May 2015, 中国铁道出版社, 第一版 *
编委会: "《溶液中金属及其他有用成分的提取》", 31 October 1995, 冶金工业出版社,第一版 *
赵俊学 等: "《冶金原理》", 30 June 2012, 冶金工业出版社,第1版 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161929A (en) * 2018-09-13 2019-01-08 浙江工业大学 A kind of method of electrodeposit metals rhenium

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