CN103604801A - Method for measuring boron content of low-grade boron ore by inductively coupled plasma atomic emission spectrometer - Google Patents
Method for measuring boron content of low-grade boron ore by inductively coupled plasma atomic emission spectrometer Download PDFInfo
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Abstract
A method for measuring boron content of low-grade boron ore by an inductively coupled plasma atomic emission spectrometer relates to a method for measuring the content of boron element in low-grade boron ore. According to the invention, the present problem that low-grade boron ore is used as compound fertilizer but there is no detection method for measuring the boron content of low-grade boron ore is solved. The method provided by the invention comprises the following steps: 1, carrying out pretreatment of a solid sample; 2, preparing a sample digestion solution and a blank digestion solution; 3, preparing a standard solution; 4, drawing a standard curve; 5, measuring the content of boron element in the sample digestion solution and the blank digestion solution; and 6, calculating the content of boron element in low-grade boron ore by a formula. Thus, measurement of the boron content in low-grade boron ore is completed by the inductively coupled plasma atomic emission spectrometer. According to the invention, the matrix interference problem of other metallic elements in low-grade boron ore is solved. The method provided by the invention has high accuracy and wide linear range. The method is applied in the field of elemental analysis.
Description
Technical field
The present invention relates to ultimate analysis field, relate generally to a kind of method of measuring boron content in low-grade boron ore.
Background technology
China's boron resource is mainly distributed in complete 14 provinces (district, city).Wherein Liaoning, Qinghai, Tibet account for respectively 64.12%%, the 29.94% and 1.44% more concentrated province of ，Shi China boron resource of national total reserves.From the fifties, first the boron industry of China rise in Liaoning, and first of the boron commercial production scale tool whole nation in Liaoning, along with the industrial development of boron, boron resource is reducing gradually.And the boron industrial development of Qinghai, Tibet region is more late, production scale also only has 1/20th of Liaoning Province.Non-renewable according to boron resource, from now on, boron industrial expansion trend must be to Qinghai, shift in Tibet.From Qinghai, the explored boron rock in two places, Tibet, mainly with lean ore, be main (B
20
3and the reserves of low-grade boron ore account for the more than 90% of this area's total reserves <16%).
In recent years, some countries that have boron resource very paid attention to the exploitation of boron resource, and the reasonable effective exploitation utilization of low-grade boron resource has become the important content of research work.Wherein for low-grade boron ore and boron mud, being applied in periodical < < phosphate fertilizer and compound fertilizer > > in fertilizer mentioned, and utilizes after low-grade boron ore and the granulation of boron mud and plays good fertilizer efficiency in application and formula fertilizer.But crop is to have quantitative limitation to the absorption of boron element, therefore understand in low-grade boron ore and boron mud boron content significant, and in existing standard GB/T/T14540-2003 in regulation complex fertilizer the assay method of boron be mainly that mensuration for boron is to take the fertilizer that borax is raw material, and as the assay method of complex fertilizer, also there is no the method for stipulating with low-grade boron ore at present.
Summary of the invention
To the object of the invention is the problem that low-grade boron ore is not had a kind of detection method measure boron content in low-grade boron ore as complex fertilizer to existing in order solving, and to provide a kind of inductively coupled plasma atomic emission spectrometer to measure the method for boron content in low-grade boron ore.
Inductively coupled plasma atomic emission spectrometer of the present invention is measured the method for boron content in low-grade boron ore, is to realize according to the following steps:
One, the pre-service of solid sample: low-grade boron ore is ground in mortar, cross 100 mesh sieves, obtain fine powder;
Two, prepare Specimen eliminating liquid and blank digestion solution:
1. the preparation of Specimen eliminating liquid: take the fine powder that 0.2～0.5g step 1 obtains and put into quartzy ground triangular flask, add 100～200mL deionized water, shake up, be placed in 200～220 ℃ of sand-bath pots, reflux condensation mode 15～20min, take off quartzy ground triangular flask, transfer in volumetric flask after being cooled to room temperature, then add 10mL red fuming nitric acid (RFNA) in volumetric flask, use deionized water constant volume, shake up, obtain digestion solution, digestion solution is filtered, discard after the 50～100mL filtrate leaching at first, retain residual filtrate, obtain Specimen eliminating liquid, for measuring boron content;
2. the preparation of blank digestion solution: in quartzy ground triangular flask, add 100～200mL deionized water, then according to step 1. described reflux condensation mode method make blank digestion solution;
Three, preparation standard solution: be that the boron standard solution that 20% salpeter solution is 1000mg/L by concentration is diluted to the boron standard solution that concentration is 100mg/L with quality percentage composition, then be the boron standard operation solution that boron standard solution stepwise dilution that 20% salpeter solution is 100mg/L by the concentration obtaining becomes 10mg/L, 8mg/L, 6mg/L, 4mg/L, 2mg/L and 0mg/L with quality percentage composition;
Four, drawing standard curve: set inductively coupled plasma atomic emission spectrometer (ICP-AES) running parameter, the boron standard operation solution of 6 concentration that obtain described in step 3 is imported in inductively coupled plasma atomic emission spectrometer, be determined at the wave spectrum intensity at 249.772nm place, the value of meeting with a response, the concentration of the boron standard operation solution of 6 concentration that the step 3 of take obtains is horizontal ordinate, the response that the inductively coupled plasma atomic emission spectrometer of take records is ordinate, draws out the standard working curve of boron element;
Wherein said inductively-coupled plasma spectrometer running parameter is: radio-frequency power 1.1KW, cooling gas flow 19L/min, integral time 10s, atomizer flow 0.35L/min, atomizer pressure is 234.5kPa, solution elevating amount 1.4mL/min, multiplicity 3 times;
Five, the content of boron element in working sample digestion solution and blank digestion solution: the Specimen eliminating liquid that step 2 is obtained and blank digestion solution import to respectively in the inductively coupled plasma atomic emission spectrometer of setting running parameter described in step 4, working sample digestion solution and blank digestion solution are in the wave spectrum intensity at 249.772nm place, obtain respectively the response of Specimen eliminating liquid and the response of blank digestion solution, the standard working curve of the boron element obtaining by step 4 again, determine the concentration of boron element in the concentration of boron element in Specimen eliminating liquid and blank digestion solution,
Six, by following formula, calculate the content of boron element in low-grade boron ore:
B (%)=(C
sample-C
blank) * V * 100%/m/1000
The mass percent of boron element in B (%)-low-grade boron ore, unit is %;
C
samplein-step 5, obtain the concentration of boron element in Specimen eliminating liquid, unit is mg/L;
C
blankin-step 5, obtain the concentration of boron element in blank digestion solution, unit is mg/L;
The capacity of the volumetric flask described in V-step 2, unit is mL;
The quality of the fine powder that the step 1 taking in m-step 2 obtains, unit is g.
Beneficial effect of the present invention:
1, the present invention adopts deionized water to boil to carry out pre-treatment, by ICP-AES method, can measure the content as boron element in complex fertilizer by low-grade boron ore, adopt ICP-AES method to measure at 249.772nm place, solved and in azomethine method, eliminated color and disturb and colour temp, the impact of developing time on result, matrix disturbs compared with causing greatly the problem that result error is larger.2, use ICP-AES standard measure to measure boron element in low-grade boron ore, the detection limit of method is between 0.005～0.09mg/L, and matrix disturbs little, can meet the needs of productive life.3, the matrix that adopts ICP-AES method can also well solve other metallic element in low-grade boron ore disturbs, and accuracy is high, and the range of linearity is wide.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the invention are not limited to this.
Embodiment one: in present embodiment, inductively coupled plasma atomic emission spectrometer is measured the method for boron content in low-grade boron ore, is to realize according to the following steps:
One, the pre-service of solid sample: low-grade boron ore is ground in mortar, cross 100 mesh sieves, obtain fine powder;
Two, prepare Specimen eliminating liquid and blank digestion solution:
1. the preparation of Specimen eliminating liquid: take the fine powder that 0.2～0.5g step 1 obtains and put into quartzy ground triangular flask, add 100～200mL deionized water, shake up, be placed in 200～220 ℃ of sand-bath pots, reflux condensation mode 15～20min, take off quartzy ground triangular flask, transfer in volumetric flask after being cooled to room temperature, then add 10mL red fuming nitric acid (RFNA) in volumetric flask, use deionized water constant volume, shake up, obtain digestion solution, digestion solution is filtered, discard after the 50～100mL filtrate leaching at first, retain residual filtrate, obtain Specimen eliminating liquid, for measuring boron content;
2. the preparation of blank digestion solution: in quartzy ground triangular flask, add 100～200mL deionized water, then according to step 1. described reflux condensation mode method make blank digestion solution;
Three, preparation standard solution: be that the boron standard solution that 20% salpeter solution is 1000mg/L by concentration is diluted to the boron standard solution that concentration is 100mg/L with quality percentage composition, then be the boron standard operation solution that boron standard solution stepwise dilution that 20% salpeter solution is 100mg/L by the concentration obtaining becomes 10mg/L, 8mg/L, 6mg/L, 4mg/L, 2mg/L and 0mg/L with quality percentage composition;
Four, drawing standard curve: set inductively coupled plasma atomic emission spectrometer running parameter, the boron standard operation solution of 6 concentration that obtain described in step 3 is imported in inductively coupled plasma atomic emission spectrometer, be determined at the wave spectrum intensity at 249.772nm place, the value of meeting with a response, the concentration of the boron standard operation solution of 6 concentration that the step 3 of take obtains is horizontal ordinate, the response that the ICP-AES spectrometer of take records is ordinate, draws out the standard working curve of boron element;
Wherein said inductively-coupled plasma spectrometer running parameter is: radio-frequency power 1.1KW, cooling gas flow 19L/min, integral time 10s, atomizer flow 0.35L/min, atomizer pressure is 234.5kPa, solution elevating amount 1.4mL/min, multiplicity 3 times;
Five, the content of boron element in working sample digestion solution and blank digestion solution: the Specimen eliminating liquid that step 2 is obtained and blank digestion solution import to respectively in the ICP-AES instrument of setting running parameter described in step 4, working sample digestion solution and blank digestion solution are in the wave spectrum intensity at 249.772nm place, obtain respectively the response of Specimen eliminating liquid and the response of blank digestion solution, the standard working curve of the boron element obtaining by step 4 again, determines the concentration of boron element in the concentration of boron element in Specimen eliminating liquid and blank digestion solution;
Six, by following formula, calculate the content of boron element in low-grade boron ore:
B (%)=(C
sample-C
blank) * V * 100%/m/1000
The mass percent of boron element in B (%)-low-grade boron ore, unit is %;
C
samplein-step 5, obtain the concentration of boron element in Specimen eliminating liquid, unit is mg/L;
C
blankin-step 5, obtain the concentration of boron element in blank digestion solution, unit is mg/L;
The capacity of the volumetric flask described in V-step 2, unit is mL;
The quality of the fine powder that the step 1 taking in m-step 2 obtains, unit is g.
Embodiment two: present embodiment is different from embodiment one, the mortar described in step 1 is that quartzy material or boron-free glass material are made.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one, the capacity of the volumetric flask described in step 2 is 250mL or 500mL.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three, the fine powder 0.2g that step 1 obtains that takes described in step 2 puts into the quartzy ground triangular flask of 250mL, adds 100mL deionized water.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four, the fine powder 0.5g that step 1 obtains that takes described in step 2 puts into the quartzy ground triangular flask of 250mL, adds 150mL deionized water.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five, and the red fuming nitric acid (RFNA) described in step 2 is analytically pure nitric acid.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six, the sand-bath pot described in step 2 is temperature control sand-bath pot.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven, the quality percentage composition described in step 3 is that 20% nitric acid is analytically pure nitric acid.Other is identical with one of embodiment one to seven.
By following verification experimental verification beneficial effect of the present invention:
This confirmatory experiment inductively coupled plasma atomic emission spectrometer is measured the method for boron content in low-grade boron ore, is to realize according to the following steps:
One, the pre-service of solid sample: low-grade boron ore is ground in mortar, cross 100 mesh sieves, obtain fine powder;
Two, prepare Specimen eliminating liquid and blank digestion solution:
1. the preparation of Specimen eliminating liquid: take the fine powder that 0.2g step 1 obtains and put into quartzy ground triangular flask, add 100mL deionized water, shake up, be placed in 200～220 ℃ of sand-bath pots, reflux condensation mode 15min, take off quartzy ground triangular flask, transfer in the volumetric flask of 250mL after being cooled to room temperature, then add 10mL red fuming nitric acid (RFNA) in volumetric flask, use deionized water constant volume, shake up, obtain 250mL digestion solution, digestion solution is filtered, discard after the 50mL filtrate leaching at first, retain residual filtrate, obtain Specimen eliminating liquid, for measuring boron content;
2. the preparation of blank digestion solution: in quartzy ground triangular flask, add 150mL deionized water, then according to step 1. described reflux condensation mode method make blank digestion solution;
Three, preparation standard solution: be that the boron standard solution that 20% salpeter solution is 1000mg/L by concentration is diluted to the boron standard solution that concentration is 100mg/L with quality percentage composition, then be the boron standard operation solution that boron standard solution stepwise dilution that 20% salpeter solution is 100mg/L by the concentration obtaining becomes 10mg/L, 8mg/L, 6mg/L, 4mg/L, 2mg/L and 0mg/L with quality percentage composition;
Four, drawing standard curve: set inductively coupled plasma atomic emission spectrometer running parameter, the boron standard operation solution of 6 concentration that obtain described in step 3 is imported in inductively coupled plasma atomic emission spectrometer, be determined at the wave spectrum intensity at 249.772nm place, the value of meeting with a response, the concentration of the boron standard operation solution of 6 concentration that the step 3 of take obtains is horizontal ordinate, the response that the ICP-AES spectrometer of take records is ordinate, draws out the standard working curve of boron element;
Wherein said inductively coupled plasma atomic emission spectrometer running parameter is: radio-frequency power 1.1KW, cooling gas flow 19L/min, integral time 10s, atomizer flow 0.35L/min, atomizer pressure is 234.5kPa, solution elevating amount 1.4mL/min, multiplicity 3 times;
Five, the content of boron element in working sample digestion solution and blank digestion solution: the Specimen eliminating liquid that step 2 is obtained and blank digestion solution import to respectively in the inductively coupled plasma atomic emission spectrometer of setting running parameter described in step 4, working sample digestion solution and blank digestion solution are in the wave spectrum intensity at 249.772nm place, obtain respectively the response of Specimen eliminating liquid and the response of blank digestion solution, the standard working curve of the boron element obtaining by step 4 again, determine the concentration of boron element in the concentration of boron element in Specimen eliminating liquid and blank digestion solution,
Six, by following formula, calculate the content of boron element in low-grade boron ore:
B (%)=(C
sample-C
blank) * V * 100%/m/1000
The mass percent of boron element in B (%)-low-grade boron ore, unit is %;
In C sample-step 5, obtain the concentration of boron element in Specimen eliminating liquid, unit is mg/L;
In C blank-step 5, obtain the concentration of boron element in blank digestion solution, unit is mg/L;
The capacity of the volumetric flask described in V-step 2, unit is mL;
The quality of the fine powder that the step 1 taking in m-step 2 obtains, unit is g.
Adopting GB/T14540-2003 and this confirmatory experiment method to measure boron content in the same low-grade boron ore of equal quality measures, multiplicity is 5 times, measurement result is as following table, mean value in table represents that same method carries out respectively replication, the mean value of 5 replication results 5 times to boron content in same low-grade boron ore.
Table one adopts GB/T14540-2003 and inductively coupled plasma atomic emission spectrometer to measure the result of boron content in the same low-grade boron ore of equal quality
Wherein GB/T14540-2003 measurement result is that 4.18%, ICP-AES measurement result is that standard variation and the relative standard deviation of 3.98%, ICP-AES method measurement result is all less than GB/T14540-2003 method, and precision is better than GB/T14540-2003.
In summary: the present invention adopts ICP-AES method to solve the matrix of other metallic element in low-grade boron ore and disturbs, accuracy is high, the range of linearity is wide, highly sensitive, can be used as existing a kind of detection method of boron content in low-grade boron ore that low-grade boron ore is measured as complex fertilizer.
Claims (7)
1. inductively coupled plasma atomic emission spectrometer is measured the method for boron content in low-grade boron ore, it is characterized in that the method for boron content in inductively coupled plasma atomic emission spectrometer mensuration low-grade boron ore, is to realize according to the following steps:
One, the pre-service of solid sample: low-grade boron ore is ground in mortar, cross 100 mesh sieves, obtain fine powder;
Two, prepare Specimen eliminating liquid and blank digestion solution:
1. the preparation of Specimen eliminating liquid: take the fine powder that 0.2～0.5g step 1 obtains and put into quartzy ground triangular flask, add 100～200mL deionized water, shake up, be placed in 200～220 ℃ of sand-bath pots, reflux condensation mode 15～20min, take off quartzy ground triangular flask, transfer in volumetric flask after being cooled to room temperature, then add 10mL red fuming nitric acid (RFNA) in volumetric flask, use deionized water constant volume, shake up, obtain digestion solution, digestion solution is filtered, discard after the 50～100mL filtrate leaching at first, retain residual filtrate, obtain Specimen eliminating liquid, for measuring boron content;
2. the preparation of blank digestion solution: in quartzy ground triangular flask, add 100～200mL deionized water, then according to step 1. described reflux condensation mode method make blank digestion solution;
Three, preparation standard solution: be that the boron standard solution that 20% salpeter solution is 1000mg/L by concentration is diluted to the boron standard solution that concentration is 100mg/L with quality percentage composition, then be the boron standard operation solution that boron standard solution stepwise dilution that 20% salpeter solution is 100mg/L by the concentration obtaining becomes 10mg/L, 8mg/L, 6mg/L, 4mg/L, 2mg/L and 0mg/L with quality percentage composition;
Four, drawing standard curve: set inductively coupled plasma atomic emission spectrometer running parameter, the boron standard operation solution of 6 concentration that obtain described in step 3 is imported in inductively coupled plasma atomic emission spectrometer, be determined at the wave spectrum intensity at 249.772nm place, the value of meeting with a response, the concentration of the boron standard operation solution of 6 concentration that the step 3 of take obtains is horizontal ordinate, the response that the inductively coupled plasma atomic emission spectrometer of take records is ordinate, draws out the standard working curve of boron element;
Wherein said inductively-coupled plasma spectrometer running parameter is: radio-frequency power 1.1KW, cooling gas flow 19L/min, integral time 10s, atomizer flow 0.35L/min, atomizer pressure is 234.5kPa, solution elevating amount 1.4mL/min, multiplicity 3 times;
Five, the content of boron element in working sample digestion solution and blank digestion solution: the Specimen eliminating liquid that step 2 is obtained and blank digestion solution import to respectively in the inductively coupled plasma atomic emission spectrometer of setting running parameter described in step 4, working sample digestion solution and blank digestion solution are in the wave spectrum intensity at 249.772nm place, obtain respectively the response of Specimen eliminating liquid and the response of blank digestion solution, the standard working curve of the boron element obtaining by step 4 again, determine the concentration of boron element in the concentration of boron element in Specimen eliminating liquid and blank digestion solution,
Six, by following formula, calculate the content of boron element in low-grade boron ore:
B (%)=(C
sample-C
blank) * V * 100%/m/1000
The mass percent of boron element in B (%)-low-grade boron ore, unit is %;
C
samplein-step 5, obtain the concentration of boron element in Specimen eliminating liquid, unit is mg/L;
C
blankin-step 5, obtain the concentration of boron element in blank digestion solution, unit is mg/L;
The capacity of the volumetric flask described in V-step 2, unit is mL;
The quality of the fine powder that the step 1 taking in m-step 2 obtains, unit is g.
2. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the mortar described in step 1 is that quartzy material or boron-free glass material are made.
3. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the fine powder 0.2g that step 1 obtains that takes described in step 2 puts into the quartzy ground triangular flask of 250mL, adds 100mL deionized water.
4. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the fine powder 0.5g that step 1 obtains that takes described in step 2 puts into the quartzy ground triangular flask of 250mL, adds 150mL deionized water.
5. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the sand-bath pot described in step 2 is temperature control sand-bath pot.
6. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the red fuming nitric acid (RFNA) described in step 2 is analytically pure nitric acid.
7. inductively coupled plasma atomic emission spectrometer according to claim 1 is measured the method for boron content in low-grade boron ore, it is characterized in that the quality percentage composition described in step 3 is that 20% nitric acid is analytically pure nitric acid.
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| CN105319203B (en) * | 2014-07-14 | 2018-07-06 | 广东先导稀材股份有限公司 | Method for measuring trace inorganic impurities in boric acid |
| CN105738346A (en) * | 2014-12-10 | 2016-07-06 | 上海宝钢工业技术服务有限公司 | Method for determining content of boron and compounds thereof in air of workplace |
| CN106814062A (en) * | 2015-11-27 | 2017-06-09 | 中冶建筑研究总院有限公司 | The method for determining various chemical element contents in slag simultaneously |
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| CN109270051A (en) * | 2018-11-27 | 2019-01-25 | 南京钢铁股份有限公司 | Use the method for Determination of Trace Boron in micro-wave digestion ICP-AES method analysis steel |
| CN109406496A (en) * | 2018-11-28 | 2019-03-01 | 中化地质矿山总局地质研究院 | Method for measuring boron content in boron ore by inductively coupled plasma emission spectrum |
| CN111504982A (en) * | 2020-04-23 | 2020-08-07 | 广州海关技术中心 | Method for measuring boron content in glass by inductively coupled plasma emission spectrometry |
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