CN102589940A

CN102589940A - Dissolving method of fluoritized phenacite and bertrandite

Info

Publication number: CN102589940A
Application number: CN2011100079448A
Authority: CN
Inventors: 汪君; 赵建新; 张建梅; 任满船; 王頔; 牛芳红; 王斌堂
Original assignee: 216 PARTY CHINA NATIONAL NUCLEAR Corp
Current assignee: 216 PARTY CHINA NATIONAL NUCLEAR Corp
Priority date: 2011-01-14
Filing date: 2011-01-14
Publication date: 2012-07-18

Abstract

The invention relates to a dissolving method of fluoritized phenacite and bertrandite, which includes the following sequential steps of: firstly, putting 0.2000g-1.000g ore sample in a polytetrafluoroethylene crucible and adding 0.2-1.0g water to wet the ore sample; secondly, sequentially adding 5.0mL-8.0mL HNO3, 10mL-15mL HF and 1.0-2.0mL HClO4 into the crucible, heating within 300 DEG C until the mixture evaporates and becomes dry, taking off and cooling to room temperature; and thirdly, adding HNO3 solution with volume ratio to the water being 1:1 into the crucible, then heating until the mixture boils and fully dissolves, taking off and cooling to room temperature, and finally adding water to dilute to get beryllium solution with acid concentration being 3-5%. According to the method of the invention, the dissolving efficiency of the phenacite and the bertrandite is improved and the process of dissolving the phenacite only lasts for two hours. Other impurities are not brought to the solution, and analysis result shows that the solution satisfies the industrial standard DZ0130-2006.

Description

The molten ore deposit method of a kind of phenakite of fluoriteization and bertrandite

Technical field

The present invention relates to a kind of molten ore deposit method of phenakite and bertrandite of fluoriteization, particularly relate to a kind of molten ore deposit method of phenakite and bertrandite of fluoriteization rapidly and efficiently.

Background technology

Since two thousand seven, along with carrying out of the applicant's beryllium ore deposit project, the quantity of beryllium sample ore article is more and more, and sample size was 856 in 2007, and sample size was 2506 in 2008, and sample size was 7707 in 2009.From above data, test center must set up the needs that accurate, efficient, the economic beryllium ore deposit analytical approach of a cover is dealt with development.Adopt the molten ore deposit of Platinum crucible in the beryllium ore deposit analytical approach of GB GB/T17414.1-98 and rower DZG93-04-two, platinum costs an arm and a leg, and operating performance simultaneously is numerous and diverse, and it is all consuming time longer that the ore deposit time is dissolved in general beryllium ore deposit, basic need 7 to 8 hours.It is slower to cause examining report to provide, and can not satisfy client and requirements of large-scale production.

Summary of the invention

The technical matters that the present invention will solve provides a kind of molten ore deposit method of phenakite and bertrandite of fluoriteization rapidly and efficiently.

For solving the problems of the technologies described above, the molten ore deposit method of the phenakite of a kind of fluoriteization of the present invention and bertrandite may further comprise the steps successively:

Step 1, get the 0.2000g-1.000g ore sample and place the teflon crucible, add 0.2g-1.0g water-wet ore sample;

Step 2, in the teflon crucible, add the HNO of 5.0mL-8.0mL successively ₃, the HF of 10mL-15mL and the HClO of 1.0-2.0mL ₄, heat with interior at 300 degrees centigrade, dried to the greatest extent until being evaporated to, take off and be cooled to room temperature;

Step 3, in the teflon crucible, to add with water volume ratio be 1: 1 HNO ₃Solution, heated and boiled is fully dissolved then, takes off and is cooled to room temperature; Thin up obtains the beryllium mineral solution then.

In the step 3, the acid concentration of beryllium mineral solution is 3-5%.

The present invention has improved the efficient in molten ore deposit, and molten at every turn ore deposit only need got final product in about 2 hours.And do not introduce other impurity, beryllium analysis on Content result in the solution is shown that its precision and accuracy meet the analysis quality requirements of the industry standard DZ0130-2006 of the People's Republic of China (PRC).

Embodiment

Embodiment one

The present invention may further comprise the steps successively:

Step 1, get the 0.2000g ore sample and place the teflon crucible, add 0.2g water-wet ore sample;

Step 2, in said teflon crucible, add the HNO of 5.0mLmL successively ₃, the HF of 10mL and the HClO of 1.0mL ₄, heat with interior at 300 degrees centigrade, dried to the greatest extent until being evaporated to, take off and be cooled to room temperature;

Step 3, in the teflon crucible, to add with water volume ratio be 1: 1 HNO ₃Solution, heated and boiled is fully dissolved then, takes off and is cooled to room temperature; To obtain acid concentration be 5% beryllium mineral solution to thin up then.

Dissolution time is 2 hours.

Draw beryllium mineral solution 2mL test solution in the 50mL volumetric flask, add 5mL mixing screening agent, mix screening agent and comprise mass ratio 5%EDTA, mass ratio 5% sodium potassium tartrate tetrahydrate and mass ratio 30% triethanolamine; Add water to 20mL, adding a concentration is the 1g/L methyl red indicator, and the HCL that drips volume ratio with water and be 1: 1 is to taking on a red color; Transfer to the NaOH solution of mass ratio 8% and just to be yellow; The HCL that adds 2.0mL mass ratio 8%, the Ai Liluo mountain valley with clumps of trees and bamboo R of 5.0mL mass ratio 0.05% shakes up 20% hexamethylenetetramine solution of CTMAB solution that the concentration that adds 2.0mL is 0.01mol/L and 5.0mL mass ratio; The rare scale that is diluted to of water shakes up.Place 90min, on spectrophotometer, do reference, measure absorbance at the 587nm place, check in corresponding beryllium content, calculate the beryllium content in the sample from working curve with the 1cm cuvette with reagent blank.Carry out measuring for 5 times that to obtain beryllium concentration respectively be 4569.5ug/g, 4701.6ug/g, 4585.1ug/g, 4592.8ug/g, 4530.7ug/g and 4631.7ug/g, mean value is 4601.9ug/g, and standard deviation RSD is 1.3%.

Embodiment two

The present invention may further comprise the steps successively:

Step 1, get the 0.500g ore sample and place the teflon crucible, add 0.5g water-wet ore sample;

Step 2, in said teflon crucible, add the HNO of 6.0mL successively ₃, the HF of 12mL and the HClO of 1.5mL ₄, heat with interior at 300 degrees centigrade, dried to the greatest extent until being evaporated to, take off and be cooled to room temperature;

Step 3, in the teflon crucible, to add with water volume ratio be 1: 1 HNO ₃Solution, heated and boiled is fully dissolved then, takes off and is cooled to room temperature; To obtain acid concentration be 3% beryllium mineral solution to thin up then.

Dissolution time is 2 hours.

Utilize plasma emission spectrometer to survey the beryllium content in the said beryllium mineral solution.Carry out measuring for 5 times that to obtain beryllium concentration respectively be 24.0ug/g, 24.0ug/g, 25.6ug/g, 27.2ug/g, 26.4ug/g and 23.3ug/g, mean value is 23.3ug/g, and standard deviation RSD is 6.2%.

Embodiment three

The present invention may further comprise the steps successively:

Step 1, get the 0.2000g-1.000g ore sample and place the teflon crucible, add 1.0g water-wet ore sample;

Step 2, in said teflon crucible, add the HNO of 8.0mL successively ₃, the HF of 15mL and the HClO of 2.0mL ₄, heat with interior at 300 degrees centigrade, dried to the greatest extent until being evaporated to, take off and be cooled to room temperature;

Step 3, in the teflon crucible, to add with water volume ratio be 1: 1 HNO ₃Solution, heated and boiled is fully dissolved then, takes off and is cooled to room temperature; To obtain acid concentration be 4% to be the beryllium mineral solution to thin up then.

Dissolution time is 2.5 hours.

Utilize plasma mass spectrograph, survey the beryllium content in the said beryllium mineral solution.Carry out measuring for 5 times that to obtain beryllium concentration respectively be 568.9ug/g, 565.0ug/g, 568.9ug/g, 573.5ug/g, 577.4ug/g and 569.6ug/g, mean value is 570.1ug/g, and standard deviation RSD is 0.8%.

Ore sample among the above embodiment all send Xinjiang Uygur Autonomous Regions's mineral products experimental study to carry out outer inspection, and the test findings error that obtains obtaining in beryllium concentration value and the present embodiment all is no more than 10%.

Claims

1. the molten ore deposit method of the phenakite of a fluoriteization and bertrandite may further comprise the steps successively:

Step 2, in said teflon crucible, add the HNO of 5.0mL-8.0mL successively ₃, the HF of 10mL-15mL and the HClO of 1.0-2.0mL ₄, heat with interior at 300 degrees centigrade, dried to the greatest extent until being evaporated to, take off and be cooled to room temperature;

2. the molten ore deposit method of the phenakite of a kind of fluoriteization according to claim 1 and bertrandite, it is characterized in that: in the said step 3, the acid concentration of said beryllium mineral solution is 3-5%.

3. the molten ore deposit method of the phenakite of a kind of fluoriteization according to claim 2 and bertrandite is characterized in that: utilize plasma emission spectrometer or plasma mass spectrograph, survey the beryllium content in the said beryllium mineral solution.