CN106093014A - Inductively coupled plasma spectrometry method quickly measures the method for rhenium content in rehenic acid ammonium - Google Patents

Inductively coupled plasma spectrometry method quickly measures the method for rhenium content in rehenic acid ammonium Download PDF

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CN106093014A
CN106093014A CN201610702846.9A CN201610702846A CN106093014A CN 106093014 A CN106093014 A CN 106093014A CN 201610702846 A CN201610702846 A CN 201610702846A CN 106093014 A CN106093014 A CN 106093014A
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volumetric flask
rhenium
solution
nitric acid
water
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CN106093014B (en
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谢明明
刘延波
雷锐
杨红忠
赵永宏
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Jinduicheng Molybdenum Co Ltd
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Abstract

The invention discloses inductively coupled plasma spectrometry method and quickly measure the method for rhenium content in rehenic acid ammonium, particularly as follows: first prepare mixed solution A, then utilize mixed solution A to prepare mixed solution B, be sequentially prepared out blank solution and four kinds of standard solution；Select spectral line, and to spectral line background process；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate；Rhenium content in rehenic acid ammonium is calculated according to algorithm.Inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content in rehenic acid ammonium, can measure rhenium content, and the advantage that technological process is succinct fast and accurately.

Description

Inductively coupled plasma spectrometry method quickly measures the method for rhenium content in rehenic acid ammonium
Technical field
The invention belongs to material assay method technical field, be specifically related to a kind of inductively coupled plasma spectrometry method quick Measure the method for rhenium content in rehenic acid ammonium.
Background technology
Rehenic acid ammonium, as the raw material of production rhenium, needs to measure the content of its rhenium metal (Re), and in rehenic acid ammonium, major constituent rhenium belongs to In high-load.
At present, assay method mainly has gravimetric method and a spectrophotography, but all to there is determination step numerous for both approaches Trivial, mensuration process is difficult to accurately control, measure the defect that interference factor is many, minute length, cost of determination are high, it is impossible to reach fast Speed and the target of low cost detection.
Inductively coupled plasma spectrometry method, as the primary analysis method of Atomic Emission Spectral Analysis method, has simple easy The feature of row, and analytical data can be provided with uncommon speed.Application inductively coupled plasma spectrometry method can realize rhenium The quick mensuration of rhenium content in acid ammonium, and there is the accurate and advantage of low cost.
Summary of the invention
It is an object of the invention to provide a kind of inductively coupled plasma spectrometry method and quickly measure rhenium content in rehenic acid ammonium Method, the content of rhenium can be measured fast and accurately, and technological process is succinct.
The technical solution adopted in the present invention is, inductively coupled plasma spectrometry method quickly measures rhenium content in rehenic acid ammonium Method, specifically according to following steps implement:
Step 1, under heating condition, rehenic acid ammonium is added in water, after rehenic acid ammonium is dissolved completely in water formed rhenium Acid ammonium solution；In Ammonium rhenate solution, add nitric acid, after boiling, be cooled to room temperature, then add dilute, obtain mixed solution A；
Step 2, measure nitric acid and the mixed solution A obtained through step 1 respectively, and by nitric acid and mixed solution A and mixing, Then add water to be diluted, obtain mixed solution B；
Step 3, after step 1 and step 2 complete, utilize water and nitric acid to prepare blank solution；
Step 4, the rhenium standard solution that concentration is 1000mg/L is carried out four kinds of dilutions in various degree, obtain four kinds of standards Solution；
Step 5, after step 4, select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and right These two spectral line backgrounds process, after process two mensuration spectral line particularly as follows: 179.312nm, left background 0.028, Right background 0；197.334nm, left background 0.0287, right background 0；
Step 6, by four kinds of standard solution obtaining through step 4 respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, measure emissive porwer at 197.334nm；Again with the mass concentration of rhenium as abscissa, with emissive porwer as vertical coordinate Draw out working curve；
Step 7, at inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure The blank solution obtained through step 3 and the emissive porwer of the mixed solution B obtained through step 2, count from corresponding working curve Calculate the concentration of the rhenium corrected through blank solution；
Step 8, calculate the content of rhenium in rehenic acid ammonium.
The feature of the present invention also resides in:
Step 1 is specifically implemented according to following steps:
Step 1.1, weigh rehenic acid ammonium 0.05g～0.5g, measure water 10mL～30mL；
Step 1.2, under heating condition, the rehenic acid ammonium weighed in step 1.1 is added in the water measured, treats rehenic acid ammonium Ammonium rhenate solution is formed after being completely dissolved in water；
Step 1.3, measure 1mL～5mL nitric acid and add in the Ammonium rhenate solution that step 1.2 obtains, obtain rehenic acid ammonium- Nitric acid mixed solution A；
Step 1.4, the rehenic acid obtained through step 1.3 ammonium-nitric acid mixed solution A is boiled after be cooled to room temperature, obtain rhenium Acid ammonium-nitric acid mixed solution B；
Step 1.5, first the rehenic acid obtained through step 1.4 ammonium-nitric acid mixed solution B is transferred to the appearance that capacity is 100mL In measuring bottle；Then in this volumetric flask, interpolation water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, is holding Mixed solution A is formed in measuring bottle.
The concentration of nitric acid is 1.42g/mL, and top grade is pure；Water uses deionized water or distilled water；Step 1.2 adds Hot temperature is: 200 DEG C～300 DEG C.
Step 2 is specifically implemented according to following steps:
Step 2.1, measure the mixed solution A that 0.50mL～2.00mL obtains through step 1；Measure 0.50mL's～2.00mL Nitric acid；
Step 2.2, the mixed solution A measured in step 2.1 is transferred to another capacity is in 100mL volumetric flask, then The nitric acid measured is also added in this volumetric flask；
Step 2.3, after step 2.2, in volumetric flask add water till reaching the 100mL graduation mark of volumetric flask, Rock volumetric flask, in volumetric flask, form mixed solution B.
In step 2.1, measure mixed solution A and use pipet or pipette, measure nitric acid and use pipette Pipe.
Concentration of nitric acid is 1.42g/mL, and top grade is pure；Water uses deionized water or distilled water.
Step 3 is specifically implemented according to following steps:
Step 3.1, measuring the water of 10mL～30mL, and heat water, heating-up temperature is 200 DEG C～300 DEG C, Xiang Shui The nitric acid of middle interpolation 1mL～5mL, forms salpeter solution；
Step 3.2, salpeter solution step 3.1 obtained are cooled to room temperature after boiling；
Step 3.3, the salpeter solution obtained through step 3.2 is transferred to a capacity is in 100mL volumetric flask, to this appearance Measuring bottle adds water, until it reaches till the 100mL graduation mark of volumetric flask, rock volumetric flask, formed blank molten in volumetric flask Liquid.
Water is distilled water or deionized water；The concentration of nitric acid is 1.42g/mL, and top grade is pure；
Step 4 is specifically implemented according to following steps:
Taking four capacity is 100mL volumetric flask, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；
In volumetric flask A, adding 2mL nitric acid, then adding water until at the 100mL graduation mark of volumetric flask A, forming titer A；
The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and adds in volumetric flask B 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask B, make all substances in volumetric flask B mix, formed Titer B；
The rhenium standard solution that 1.00mL concentration is 1000mg/L is added in volumetric flask C, and adds in volumetric flask C 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask C, make all substances in volumetric flask C mix, formed Titer C；
The rhenium standard solution that 2.00mL concentration is 1000mg/L is added in volumetric flask D, and adds in volumetric flask D 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask D, make the rhenium standard solution in volumetric flask D mix with water Even, form titer D；
The concentration of nitric acid is 1.42g/mL, and top grade is pure；The water added is deionized water or distilled water.
Algorithm in step 8 is specific as follows:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate.
The beneficial effects of the present invention is:
(1) inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content in rehenic acid ammonium, can quickly and Determine the content of rhenium accurately, especially can quickly measure the rehenic acid ammonium that rhenium content is higher.
(2) inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content in rehenic acid ammonium, and it measures Accuracy and precision are the highest.
(3) inductively coupled plasma spectrometry method of the present invention quickly measure the method for rhenium content in rehenic acid ammonium have operation letter Just, efficiency is high, effective, pollute little advantage, can be used for production process control and finished product detection.
(4) inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content, application prospect in rehenic acid ammonium Extensively, the requirement that rhenium content in rehenic acid ammonium product is quickly detected by research and production can be met.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
Inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content in rehenic acid ammonium, specifically according to following Step is implemented:
Step 1, under heating condition, rehenic acid ammonium is added in water, after rehenic acid ammonium is dissolved completely in water formed rhenium Acid ammonium solution；In Ammonium rhenate solution, add nitric acid, after boiling, be cooled to room temperature, then add dilute, obtain mixed solution A, specifically implements according to following steps:
Step 1.1, weigh rehenic acid ammonium 0.05g～0.5g (being accurate to 0.0001g when weighing), measure water 10mL～30mL, (can be contained in beaker standby)；
Wherein, water uses deionized water or distilled water；
Step 1.2, under heating condition, the rehenic acid ammonium weighed in step 1.1 is added in the water measured, treats rehenic acid ammonium Ammonium rhenate solution is formed after being completely dissolved in water；
Wherein, heating-up temperature is: 200 DEG C～300 DEG C；
Step 1.3, measure 1mL～5mL nitric acid and add in the Ammonium rhenate solution that step 1.2 obtains, obtain rehenic acid ammonium- Nitric acid mixed solution A；
Wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；
Step 1.4, the rehenic acid obtained through step 1.3 ammonium-nitric acid mixed solution A is boiled after be cooled to room temperature, obtain rhenium Acid ammonium-nitric acid mixed solution B；
Step 1.5, first the rehenic acid obtained through step 1.4 ammonium-nitric acid mixed solution B is transferred to the appearance that capacity is 100mL In measuring bottle；Then in this volumetric flask, interpolation water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, is holding Mixed solution A is formed in measuring bottle.
Step 2, measure nitric acid and the mixed solution A obtained through step 1 respectively, and by nitric acid and mixed solution A and mixing, Then add water to be diluted, obtain mixed solution B, specifically implement according to following steps:
Step 2.1, measure the mixed solution A that 0.50mL～2.00mL obtains through step 1；Measure 0.50mL's～2.00mL Nitric acid；
Wherein, measure mixed solution A and use pipet or pipette, measure nitric acid and use pipette；
Concentration of nitric acid is 1.42g/mL, and top grade is pure；
Step 2.2, the mixed solution A measured in step 2.1 is transferred to another capacity is in 100mL volumetric flask, then The nitric acid measured is also added in this volumetric flask；
Step 2.3, after step 2.2, in volumetric flask add water till reaching the 100mL graduation mark of volumetric flask, Rock volumetric flask, in volumetric flask, form mixed solution B；
Water uses deionized water or distilled water.
Step 3, after step 1 and step 2 complete, utilize water and nitric acid to prepare blank solution, specifically according to following step Rapid enforcement:
Step 3.1, measuring the water (being placed in beaker) of 10mL～30mL, and water is carried out heat treated, heating-up temperature is 200 DEG C～300 DEG C；Xiang Shuizhong adds the nitric acid of 1mL～5mL, forms salpeter solution；
Wherein, water used is distilled water or deionized water；
The concentration of nitric acid is 1.42g/mL, and top grade is pure；
Step 3.2, salpeter solution step 3.1 obtained are cooled to room temperature after boiling；
Step 3.3, the salpeter solution obtained through step 3.2 is transferred to a capacity is in 100mL volumetric flask, to this appearance Measuring bottle adds water, until it reaches till the 100mL graduation mark of volumetric flask, formed blank molten after rocking volumetric flask in volumetric flask Liquid.
Step 4, rhenium standard solution that concentration is 1000mg/L (is bought and surveyed in country's non-ferrous metal and electronic material analysis Examination center, national standard sample) carry out four kinds of dilutions in various degree, obtain four kinds of standard solution, the most in accordance with the following methods Implement:
Taking four capacity is 100mL volumetric flask, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；
In volumetric flask A, adding 2mL nitric acid, then adding water until at the 100mL graduation mark of volumetric flask A, forming titer A；
The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and adds in volumetric flask B 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask B, make all substances in volumetric flask B mix, formed Titer B；
The rhenium standard solution that 1.00mL concentration is 1000mg/L is added in volumetric flask C, and adds in volumetric flask C 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask C, make all substances in volumetric flask C mix, formed Titer C；
The rhenium standard solution that 2.00mL concentration is 1000mg/L is added in volumetric flask D, and adds in volumetric flask D 2mL nitric acid, then add water until reaching at the 100mL graduation mark of volumetric flask D, make the rhenium standard solution in volumetric flask D mix with water Even, form titer D.
Wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；The water used is deionized water or distilled water.
Step 5, after step 4, select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and right These two spectral line backgrounds process, after process two mensuration spectral line particularly as follows: 179.312nm, left background 0.028, Right background 0；197.334nm, left background 0.0287, right background 0.
Step 6, by four kinds of standard solution obtaining through step 4 respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, measure emissive porwer at 197.334nm；Again with the mass concentration of rhenium as abscissa, with emissive porwer as vertical coordinate Draw out working curve.
Step 7, at inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure The blank solution obtained through step 3 and the emissive porwer of the mixed solution B obtained through step 2, count from corresponding working curve Calculate the concentration of the rhenium corrected through blank solution.
Step 8, calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate.
Embodiment 1
Weigh rehenic acid ammonium 0.05g (being accurate to 0.0001g), measure deionized water 10mL and be placed in beaker；In 200 DEG C of heating Under the conditions of, the rehenic acid ammonium weighed is added in the water measured, after rehenic acid ammonium is completely dissolved in deionized water, forms rehenic acid Ammonium salt solution；Measure 1mL nitric acid and add in Ammonium rhenate solution, obtain rehenic acid ammonium-nitric acid mixed solution A, wherein, the concentration of nitric acid For 1.42g/mL, top grade is pure；It is cooled to room temperature after rehenic acid ammonium-nitric acid mixed solution A being boiled, obtains rehenic acid ammonium-nitric acid mixing Solution B；First rehenic acid ammonium-nitric acid mixed solution B is transferred in the volumetric flask that capacity is 100mL, then adds in this volumetric flask Add deionized water till reaching the 100mL graduation mark of volumetric flask, rock volumetric flask, in volumetric flask, form mixed solution A；
Measure the mixed solution A of 0.50mL (being accurate to 0.01mL) with pipette, measure the nitric acid of 0.50mL, wherein nitric acid Concentration is 1.42g/mL, and top grade is pure；It is in 100mL volumetric flask that the mixed solution A measured is transferred to another capacity, then will amount The nitric acid taken is also added in this volumetric flask；Deionized water is added until reaching the 100mL graduation mark of volumetric flask in volumetric flask Till, rock volumetric flask, in volumetric flask, form mixed solution B；
Measure the deionized water of 10mL, and by deionized water in 200 DEG C of heated and boiled；In deionized water, add 1mL's Nitric acid, forms salpeter solution, and the concentration of nitric acid is 1.42g/mL, and top grade is pure；Room temperature it is cooled to after being boiled by salpeter solution；By nitre It is in 100mL volumetric flask that acid solution is transferred to a capacity, adds deionized water, until it reaches volumetric flask in this volumetric flask Till 100mL graduation mark, rock volumetric flask, in volumetric flask, form blank solution；
Measure the rhenium standard solution that 0.50mL, 1.00mL, 2.00mL (being accurate to 0.01mL) concentration is 1000mg/L respectively (buying in country's non-ferrous metal and electronic material Institute of Analysis, national standard sample)；Taking four capacity is 100mL capacity Bottle, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；In volumetric flask A, add 2mL nitric acid, then interpolation is gone Ionized water until volumetric flask A 100mL graduation mark at, formed titer A, wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add deionized water until reaching at the 100mL graduation mark of volumetric flask B, make rhenium standard solution in volumetric flask B with go from Sub-water mixes, and forms titer B, and wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；It is 1000mg/L by 1.00mL concentration Rhenium standard solution add in volumetric flask C, and in volumetric flask C add 2mL nitric acid, then add deionized water until reach hold At the 100mL graduation mark of measuring bottle C, the rhenium standard solution in volumetric flask C is made to mix with deionized water, formation titer C, wherein, The concentration of nitric acid is 1.42g/mL, and top grade is pure；Add the rhenium standard solution that 2.00mL concentration is 1000mg/L to volumetric flask D In, and in volumetric flask D, add 2mL nitric acid, then add deionized water until reaching, at the 100mL graduation mark of volumetric flask D, to make appearance Rhenium standard solution in measuring bottle D mixes with deionized water, forms titer D, and wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；
Select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and to these two spectral line backgrounds Processing, two mensuration spectral line after process are specific as follows: 179.312nm, left background 0.028, right background 0； 197.334nm, left background 0.0287, right background 0；
By four kinds of standard solution respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, 197.334nm Place measures emissive porwer；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate； 197.312nm spectral line working curve linear equation is I=0.00001519C-0.03239, and linearly dependent coefficient is 0.9999； 197.334nm spectral line working curve linear equation is I=0.00001507C-0.0175, linearly dependent coefficient 0.9999；
At inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step 3 The blank solution obtained and the emissive porwer of the mixed solution B obtained through step 2, calculate through blank from corresponding working curve The concentration of the rhenium of solution correction；
Calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate；Measurement result is: 67.03% (197.312nm), 67.08% (197.334nm).
Embodiment 2
Weigh rehenic acid ammonium 0.1g (being accurate to 0.0001g), measure distilled water 15mL and be placed in beaker；In 230 DEG C of fire-bars Under part, the rehenic acid ammonium weighed is added in the water measured, after rehenic acid ammonium is completely dissolved in distilled water, form rehenic acid ammonium molten Liquid；Measuring 2mL nitric acid and add in Ammonium rhenate solution, obtain rehenic acid ammonium-nitric acid mixed solution A, wherein, the concentration of nitric acid is 1.42g/mL, top grade is pure；It is cooled to room temperature after rehenic acid ammonium-nitric acid mixed solution A being boiled, obtains rehenic acid ammonium-nitric acid mixing molten Liquid B；First rehenic acid ammonium-nitric acid mixed solution B is transferred in the volumetric flask that capacity is 100mL, then adds in this volumetric flask Distilled water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, forms mixed solution A in volumetric flask；
Measure the mixed solution A of 1.00mL (being accurate to 0.01mL) with pipet, measure the nitric acid of 1.00mL, wherein nitric acid Concentration is 1.42g/mL, and top grade is pure；It is in 100mL volumetric flask that the mixed solution A measured is transferred to another capacity, then will amount The nitric acid taken is also added in this volumetric flask；Distilled water is added until the 100mL graduation mark reaching volumetric flask is in volumetric flask Only, rock volumetric flask, in volumetric flask, form mixed solution B；
Measure the distilled water of 15mL, and by distilled water in 230 DEG C of heated and boiled；The nitric acid of 2mL, shape is added in distilled water Becoming salpeter solution, the concentration of nitric acid is 1.42g/mL, and top grade is pure；Room temperature it is cooled to after being boiled by salpeter solution；By salpeter solution Being transferred to a capacity is in 100mL volumetric flask, adds distilled water, until it reaches the 100mL of volumetric flask carves in this volumetric flask Till degree line, rock volumetric flask, in volumetric flask, form blank solution；
Measure the rhenium standard solution that 0.50mL, 1.00mL, 2.00mL (being accurate to 0.01mL) concentration is 1000mg/L respectively (buying in country's non-ferrous metal and electronic material Institute of Analysis, national standard sample)；Taking four capacity is 100mL capacity Bottle, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；In volumetric flask A, add 2mL nitric acid, then interpolation is gone Ionized water until volumetric flask A 100mL graduation mark at, formed titer A, wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add deionized water until reaching at the 100mL graduation mark of volumetric flask B, make rhenium standard solution in volumetric flask B with go from Sub-water mixes, and forms titer B, and wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；It is 1000mg/L by 1.00mL concentration Rhenium standard solution add in volumetric flask C, and in volumetric flask C add 2mL nitric acid, then add deionized water until reach hold At the 100mL graduation mark of measuring bottle C, the rhenium standard solution in volumetric flask C is made to mix with deionized water, formation titer C, wherein, The concentration of nitric acid is 1.42g/mL, and top grade is pure；Add the rhenium standard solution that 2.00mL concentration is 1000mg/L to volumetric flask D In, and in volumetric flask D, add 2mL nitric acid, then add deionized water until reaching, at the 100mL graduation mark of volumetric flask D, to make appearance Rhenium standard solution in measuring bottle D mixes with deionized water, forms titer D, and wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；
Select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and to these two spectral line backgrounds Processing, two mensuration spectral line after process are specific as follows: 179.312nm, left background 0.028, right background 0； 197.334nm, left background 0.0287, right background 0；
By four kinds of standard solution respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, 197.334nm Place measures emissive porwer；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate； 197.312nm spectral line working curve linear equation is I=0.00001519C-0.03239, and linearly dependent coefficient is 0.9999. 197.334nm spectral line working curve linear equation is I=0.00001507C-0.0175, linearly dependent coefficient 0.9999；
At inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step 3 The blank solution obtained and the emissive porwer of the mixed solution B obtained through step 2, calculate through blank from corresponding working curve The concentration of the rhenium of solution correction；
Calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate；Measurement result is: 69.02% (197.312nm), 69.03% (197.334nm).
Embodiment 3
Weigh rehenic acid ammonium 0.2g (being accurate to 0.0001g), measure distilled water 20mL and be placed in beaker；In 250 DEG C of fire-bars Under part, the rehenic acid ammonium weighed is added in the water measured, after rehenic acid ammonium is completely dissolved in distilled water, form rehenic acid ammonium molten Liquid；Measuring 3mL nitric acid and add in Ammonium rhenate solution, obtain rehenic acid ammonium-nitric acid mixed solution A, wherein, the concentration of nitric acid is 1.42g/mL, top grade is pure；It is cooled to room temperature after rehenic acid ammonium-nitric acid mixed solution A being boiled, obtains rehenic acid ammonium-nitric acid mixing molten Liquid B；First rehenic acid ammonium-nitric acid mixed solution B is transferred in the volumetric flask that capacity is 100mL, then adds in this volumetric flask Distilled water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, is the formation of mixed solution A in volumetric flask；
Measure the mixed solution A of 1.00mL (being accurate to 0.01mL) with pipet, measure the nitric acid of 1.00mL, wherein nitric acid Concentration is 1.42g/mL, and top grade is pure；It is in 100mL volumetric flask that the mixed solution A measured is transferred to another capacity, then will amount The nitric acid taken is also added in this volumetric flask；Distilled water is added until the 100mL graduation mark reaching volumetric flask is in volumetric flask Only, rock volumetric flask, in volumetric flask, form mixed solution B；
Measure the distilled water of 20mL, and distilled water is heated to 250 DEG C；In distilled water, add the nitric acid of 3mL, form nitre Acid solution, the concentration of nitric acid is 1.42g/mL, and top grade is pure；Room temperature it is cooled to after being boiled by salpeter solution；Salpeter solution is shifted It is in 100mL volumetric flask to a capacity, in this volumetric flask, adds distilled water, until it reaches the 100mL graduation mark of volumetric flask Till, rock volumetric flask, in volumetric flask, form blank solution；
Measure the rhenium standard solution that 0.50mL, 1.00mL, 2.00mL (being accurate to 0.01mL) concentration is 1000mg/L respectively (buying in country's non-ferrous metal and electronic material Institute of Analysis, national standard sample)；Taking four capacity is 100mL capacity Bottle, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；In volumetric flask A, add 2mL nitric acid, then interpolation is gone Ionized water until volumetric flask A 100mL graduation mark at, formed titer A, wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add deionized water until reaching at the 100mL graduation mark of volumetric flask B, make rhenium standard solution in volumetric flask B with go from Sub-water mixes, and forms titer B, and wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；It is 1000mg/L by 1.00mL concentration Rhenium standard solution add in volumetric flask C, and in volumetric flask C add 2mL nitric acid, then add deionized water until reach hold At the 100mL graduation mark of measuring bottle C, the rhenium standard solution in volumetric flask C is made to mix with deionized water, formation titer C, wherein, The concentration of nitric acid is 1.42g/mL, and top grade is pure；Add the rhenium standard solution that 2.00mL concentration is 1000mg/L to volumetric flask D In, and in volumetric flask D, add 2mL nitric acid, then add deionized water until reaching, at the 100mL graduation mark of volumetric flask D, to make appearance Rhenium standard solution in measuring bottle D mixes with deionized water, forms titer D, and wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；
Select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and to these two spectral line backgrounds Processing, two mensuration spectral line after process are specific as follows: 179.312nm, left background 0.028, right background 0； 197.334nm, left background 0.0287, right background 0；
By four kinds of standard solution respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, 197.334nm Place measures emissive porwer；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate； 197.312nm spectral line working curve linear equation is I=0.00001519C-0.03239, and linearly dependent coefficient is 0.9999. 197.334nm spectral line working curve linear equation is I=0.00001507C-0.0175, linearly dependent coefficient 0.9999；
At inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step 3 The blank solution obtained and the emissive porwer of the mixed solution B obtained through step 2, calculate through blank from corresponding working curve The concentration of the rhenium of solution correction；
Calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate；Measurement result is: 60.32% (197.312nm), 60.56% (197.334nm).
Embodiment 4
Weigh rehenic acid ammonium 0.3g (being accurate to 0.0001g), measure distilled water 25mL and be placed in beaker；In 280 DEG C of fire-bars Under part, the rehenic acid ammonium weighed is added in the water measured, after rehenic acid ammonium is completely dissolved in distilled water, form rehenic acid ammonium molten Liquid；Measuring 4mL nitric acid and add in Ammonium rhenate solution, obtain rehenic acid ammonium-nitric acid mixed solution A, wherein, the concentration of nitric acid is 1.42g/mL, top grade is pure；It is cooled to room temperature after rehenic acid ammonium-nitric acid mixed solution A being boiled, obtains rehenic acid ammonium-nitric acid mixing molten Liquid B；First rehenic acid ammonium-nitric acid mixed solution B is transferred in the volumetric flask that capacity is 100mL, then adds in this volumetric flask Distilled water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, is the formation of mixed solution A in volumetric flask；
Measure the mixed solution A of 1.50mL (being accurate to 0.01mL) with pipette, measure the nitric acid of 1.50mL, wherein nitric acid Concentration is 1.42g/mL, and top grade is pure；It is in 100mL volumetric flask that the mixed solution A measured is transferred to another capacity, then will amount The nitric acid taken is also added in this volumetric flask；Distilled water is added until the 100mL graduation mark reaching volumetric flask is in volumetric flask Only, rock volumetric flask, in volumetric flask, form mixed solution B；
Measure the distilled water of 25mL, and distilled water is heated to 280 DEG C；In distilled water, add the nitric acid of 4mL, form nitre Acid solution, the concentration of nitric acid is 1.42g/mL, and top grade is pure；Room temperature it is cooled to after being boiled by salpeter solution；Salpeter solution is shifted It is in 100mL volumetric flask to a capacity, in this volumetric flask, adds distilled water, until it reaches the 100mL graduation mark of volumetric flask Till, rock volumetric flask, in volumetric flask, form blank solution；
Measure the rhenium standard solution that 0.50mL, 1.00mL, 2.00mL (being accurate to 0.01mL) concentration is 1000mg/L respectively (buying in country's non-ferrous metal and electronic material Institute of Analysis, national standard sample)；Taking four capacity is 100mL capacity Bottle, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；In volumetric flask A, add 2mL nitric acid, then interpolation is gone Ionized water until volumetric flask A 100mL graduation mark at, formed titer A, wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add deionized water until reaching at the 100mL graduation mark of volumetric flask B, make rhenium standard solution in volumetric flask B with go from Sub-water mixes, and forms titer B, and wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；It is 1000mg/L by 1.00mL concentration Rhenium standard solution add in volumetric flask C, and in volumetric flask C add 2mL nitric acid, then add deionized water until reach hold At the 100mL graduation mark of measuring bottle C, the rhenium standard solution in volumetric flask C is made to mix with deionized water, formation titer C, wherein, The concentration of nitric acid is 1.42g/mL, and top grade is pure；Add the rhenium standard solution that 2.00mL concentration is 1000mg/L to volumetric flask D In, and in volumetric flask D, add 2mL nitric acid, then add deionized water until reaching, at the 100mL graduation mark of volumetric flask D, to make appearance Rhenium standard solution in measuring bottle D mixes with deionized water, forms titer D, and wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；
Select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and to these two spectral line backgrounds Processing, two mensuration spectral line after process are specific as follows: 179.312nm, left background 0.028, right background 0； 197.334nm, left background 0.0287, right background 0；
By four kinds of standard solution respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, 197.334nm Place measures emissive porwer；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate； 197.312nm spectral line working curve linear equation is I=0.00001519C-0.03239, and linearly dependent coefficient is 0.9999. 197.334nm spectral line working curve linear equation is I=0.00001507C-0.0175, linearly dependent coefficient 0.9999；
At inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step 3 The blank solution obtained and the emissive porwer of the mixed solution B obtained through step 2, calculate through blank from corresponding working curve The concentration of the rhenium of solution correction；
Calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate；Measurement result is: 55.94% (197.312nm), 56.02% (197.334nm).
Embodiment 5
Weigh rehenic acid ammonium 0.5g (being accurate to 0.0001g), measure deionized water 30mL and be placed in beaker；In 300 DEG C of heating Under the conditions of, the rehenic acid ammonium weighed is added in the water measured, after rehenic acid ammonium is completely dissolved in deionized water, forms rehenic acid Ammonium salt solution；Measure 5mL nitric acid and add in Ammonium rhenate solution, obtain rehenic acid ammonium-nitric acid mixed solution A, wherein, the concentration of nitric acid For 1.42g/mL, top grade is pure；It is cooled to room temperature after rehenic acid ammonium-nitric acid mixed solution A being boiled, obtains rehenic acid ammonium-nitric acid mixing Solution B；First rehenic acid ammonium-nitric acid mixed solution B is transferred in the volumetric flask that capacity is 100mL, then adds in this volumetric flask Add deionized water till reaching the 100mL graduation mark of volumetric flask, rock volumetric flask, in volumetric flask, define mixed solution A；
Measuring the mixed solution A of 2mL (being accurate to 0.01mL) with pipet, measure the nitric acid of 2mL, wherein concentration of nitric acid is 1.42g/mL, top grade is pure；It is in 100mL volumetric flask that the mixed solution A measured is transferred to another capacity, then the nitre that will measure Acid is also added in this volumetric flask；In volumetric flask, interpolation deionized water is till reaching the 100mL graduation mark of volumetric flask, shakes Rolling volumetric flask, forms mixed solution B in volumetric flask；
Measure the deionized water of 30mL, and by deionized water in 300 DEG C of heated and boiled；In deionized water, add 1mL's Nitric acid, forms salpeter solution, and the concentration of nitric acid is 1.42g/mL, and top grade is pure；Room temperature it is cooled to after being boiled by salpeter solution；By nitre It is in 100mL volumetric flask that acid solution is transferred to a capacity, adds deionized water, until it reaches volumetric flask in this volumetric flask Till 100mL graduation mark, in volumetric flask, after rocking volumetric flask, form blank solution；
Measure the rhenium standard solution that 0.50mL, 1.00mL, 2.00mL (being accurate to 0.01mL) concentration is 1000mg/L respectively (buying in country's non-ferrous metal and electronic material Institute of Analysis, national standard sample)；Taking four capacity is 100mL capacity Bottle, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；In volumetric flask A, add 2mL nitric acid, then interpolation is gone Ionized water until volumetric flask A 100mL graduation mark at, formed titer A, wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add deionized water until reaching at the 100mL graduation mark of volumetric flask B, make rhenium standard solution in volumetric flask B with go from Sub-water mixes, and forms titer B, and wherein, the concentration of nitric acid is 1.42g/mL, and top grade is pure；It is 1000mg/L by 1.00mL concentration Rhenium standard solution add in volumetric flask C, and in volumetric flask C add 2mL nitric acid, then add deionized water until reach hold At the 100mL graduation mark of measuring bottle C, the rhenium standard solution in volumetric flask C is made to mix with deionized water, formation titer C, wherein, The concentration of nitric acid is 1.42g/mL, and top grade is pure；Add the rhenium standard solution that 2.00mL concentration is 1000mg/L to volumetric flask D In, and in volumetric flask D, add 2mL nitric acid, then add deionized water until reaching, at the 100mL graduation mark of volumetric flask D, to make appearance Rhenium standard solution in measuring bottle D mixes with deionized water, forms titer D, and wherein, the concentration of nitric acid is 1.42g/mL, top grade Pure；
Select two spectral line of 197.312nm and 197.334nm as measuring spectral line, and to these two spectral line backgrounds Processing, two mensuration spectral line after process are specific as follows: 179.312nm, left background 0.028, right background 0； 197.334nm, left background 0.0287, right background 0；
By four kinds of standard solution respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, 197.334nm Place measures emissive porwer；With the mass concentration of rhenium as abscissa, draw out working curve with emissive porwer for vertical coordinate； 197.312nm spectral line working curve linear equation is I=0.00001519C-0.03239, and linearly dependent coefficient is 0.9999. 197.334nm spectral line working curve linear equation is I=0.00001507C-0.0175, linearly dependent coefficient 0.9999.
At inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step 3 The blank solution obtained and the emissive porwer of the mixed solution B obtained through step 2, calculate through blank from corresponding working curve The concentration of the rhenium of solution correction；
Calculate the content of rhenium in rehenic acid ammonium, specifically implement according to following algorithm:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is from working song The concentration of rhenium in the blank solution checked on line, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, Unit is g；D-extension rate；Measurement result is: 50.13% (197.312nm), 50.36% (197.334nm).
Inductively coupled plasma spectrometry method of the present invention quickly measures the method for rhenium content in rehenic acid ammonium, can be quickly with accurate Mensuration rhenium content, and technological process is succinct.

Claims (10)

1. the method for rhenium content during inductively coupled plasma spectrometry method quickly measures rehenic acid ammonium, it is characterised in that specifically according to Following steps are implemented:
Step 1, under heating condition, rehenic acid ammonium is added in water, after rehenic acid ammonium is dissolved completely in water formed rehenic acid ammonium Solution；In Ammonium rhenate solution, add nitric acid, after boiling, be cooled to room temperature, then add dilute, obtain mixed solution A；
Step 2, measure nitric acid and the mixed solution A obtained through step 1 respectively, and by nitric acid and mixed solution A and mixing, then Add water to be diluted, obtain mixed solution B；
Step 3, after step 1 and step 2 complete, utilize water and nitric acid to prepare blank solution；
Step 4, the rhenium standard solution that concentration is 1000mg/L is carried out four kinds of dilutions in various degree, obtain four kinds of standards molten Liquid；
Step 5, after step 4, select two spectral line of 197.312nm and 197.334nm as measure spectral line, and to this two Bar spectral line background processes, and after process two mensuration spectral line are particularly as follows: 179.312nm, left background 0.028, the right back of the body Scape 0；197.334nm, left background 0.0287, right background 0；
Step 6, by four kinds of standard solution obtaining through step 4 respectively at inductive coupling plasma emission spectrograph wavelength 179.312nm, measure emissive porwer at 197.334nm；Again with the mass concentration of rhenium as abscissa, with emissive porwer as vertical coordinate Draw out working curve；
Step 7, at inductively coupled plasma atomic emission spectrometer wavelength 179.312nm, 197.334nm, measure through step Rapid 3 blank solutions obtained and the emissive porwer of mixed solution B obtained through step 2, calculate warp from corresponding working curve The concentration of the rhenium of blank solution correction；
Step 8, calculate the content of rhenium in rehenic acid ammonium.
Inductively coupled plasma spectrometry method the most according to claim 1 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described step 1 is specifically implemented according to following steps:
Step 1.1, weigh rehenic acid ammonium 0.05g～0.5g, measure water 10mL～30mL；
Step 1.2, under heating condition, the rehenic acid ammonium weighed in step 1.1 is added in the water measured, treats that rehenic acid ammonium is complete Ammonium rhenate solution is formed after being dissolved in water；
Step 1.3, measure 1mL～5mL nitric acid and add in the Ammonium rhenate solution that step 1.2 obtains, obtain rehenic acid ammonium-nitric acid Mixed solution A；
Step 1.4, the rehenic acid obtained through step 1.3 ammonium-nitric acid mixed solution A is boiled after be cooled to room temperature, obtain rehenic acid ammonium- Nitric acid mixed solution B；
Step 1.5, first the rehenic acid obtained through step 1.4 ammonium-nitric acid mixed solution B is transferred to the volumetric flask that capacity is 100mL In；Then in this volumetric flask, interpolation water, till reaching the 100mL graduation mark of volumetric flask, rocks volumetric flask, at volumetric flask Interior formation mixed solution A.
Inductively coupled plasma spectrometry method the most according to claim 2 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, the concentration of described nitric acid is 1.42g/mL, and top grade is pure；Described water uses deionized water or distilled water；
In described step 1.2, heating-up temperature is: 200 DEG C～300 DEG C.
Inductively coupled plasma spectrometry method the most according to claim 1 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described step 2 is specifically implemented according to following steps:
Step 2.1, measure the mixed solution A that 0.50mL～2.00mL obtains through step 1；Measure the nitre of 0.50mL～2.00mL Acid；
Step 2.2, the mixed solution A measured in step 2.1 is transferred to another capacity is in 100mL volumetric flask, then will amount The nitric acid taken is also added in this volumetric flask；
Step 2.3, after step 2.2, in volumetric flask add water till reaching the 100mL graduation mark of volumetric flask, rock Volumetric flask, forms mixed solution B in volumetric flask.
Inductively coupled plasma spectrometry method the most according to claim 4 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, in described step 2.1, measure mixed solution A and use pipet or pipette, measure what nitric acid used It it is pipette.
Inductively coupled plasma spectrometry method the most according to claim 4 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described concentration of nitric acid is 1.42g/mL, and top grade is pure；Described water uses deionized water or distilled water.
Inductively coupled plasma spectrometry method the most according to claim 1 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described step 3 is specifically implemented according to following steps:
Step 3.1, measuring the water of 10mL～30mL, and heat water, heating-up temperature is 200 DEG C～300 DEG C, adds in water Add the nitric acid of 1mL～5mL, form salpeter solution；
Step 3.2, salpeter solution step 3.1 obtained are cooled to room temperature after boiling；
Step 3.3, the salpeter solution obtained through step 3.2 is transferred to a capacity is in 100mL volumetric flask, to this volumetric flask Middle interpolation water, until it reaches till the 100mL graduation mark of volumetric flask, rock volumetric flask, forms blank solution in volumetric flask.
Inductively coupled plasma spectrometry method the most according to claim 7 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described water is distilled water or deionized water；The concentration of nitric acid is 1.42g/mL, and top grade is pure.
Inductively coupled plasma spectrometry method the most according to claim 1 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, described step 4 is specifically implemented according to following steps:
Taking four capacity is 100mL volumetric flask, is respectively labeled as volumetric flask A, volumetric flask B, volumetric flask C, volumetric flask D；
In volumetric flask A, adding 2mL nitric acid, then adding water until at the 100mL graduation mark of volumetric flask A, forming titer A；
The rhenium standard solution that 0.50mL concentration is 1000mg/L is added in volumetric flask B, and in volumetric flask B, adds 2mL nitre Acid, then add water until reaching at the 100mL graduation mark of volumetric flask B, make all substances in volumetric flask B mix, form standard Liquid B；
The rhenium standard solution that 1.00mL concentration is 1000mg/L is added in volumetric flask C, and in volumetric flask C, adds 2mL nitre Acid, then add water until reaching at the 100mL graduation mark of volumetric flask C, make all substances in volumetric flask C mix, form standard Liquid C；
The rhenium standard solution that 2.00mL concentration is 1000mg/L is added in volumetric flask D, and in volumetric flask D, adds 2mL nitre Acid, then add water until reaching at the 100mL graduation mark of volumetric flask D, make the rhenium standard solution in volumetric flask D mix with water, shape Become titer D；
The concentration of nitric acid is 1.42g/mL, and top grade is pure；The water added is deionized water or distilled water.
Inductively coupled plasma spectrometry method the most according to claim 1 quickly measures the method for rhenium content in rehenic acid ammonium, It is characterized in that, the algorithm in described step 8 is specific as follows:
In rehenic acid ammonium, rhenium content is with the mass fraction w of rheniumReMeter, numerical value represents with %, implements by following algorithm:
w V = ( ρ 1 - ρ 2 ) · V × 10 - 6 × d m × 100 ;
In formula: what ρ 1-checked on working curve measures the concentration of rhenium in solution, and unit is μ g/mL；ρ 2-is on working curve The concentration of rhenium in the blank solution checked in, unit is μ g/mL；V-test solution cumulative volume, unit is mL；The quality of m-test portion, unit For g；D-extension rate.
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