CN108362684A - The analysis method of gallium element in a kind of measurement rafifinal - Google Patents
The analysis method of gallium element in a kind of measurement rafifinal Download PDFInfo
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Abstract
The invention belongs to high pure metal trace element analysis technologies, are related to a kind of analysis method measuring gallium in rafifinal.The present invention is dissolved sample using 10mL~20mL hydrochloric acid (1+1), 3mL~8mL nitric acid, heating is added.The present invention dissolves sample with dilute hydrochloric acid, nitric acid, to obtain clear sample solution；By carrying out interference experiment, it is determined that optimized analysis spectral line improves the accuracy of measurement；Method measurement range is wide, and it is 0.0005% to measure offline, and it is 0.005% to measure the upper limit；Using synchronization process sample and calibration solution measurement gallium element is prepared, analytical error is minimum, and method is reproducible；The rate of recovery, precision are preferable；Show that made fixed analysis method accuracy is good by analysis results comparisons such as the analysis of standard sample, method reinspections, method is stablized, and the requirement of trace element analysis is complied fully with；The method of the present invention measures quickly, easy to operate, has saved a large amount of man power and materials.
Description
Technical field
The invention belongs to high pure metal trace element analysis technologies, are related to a kind of analysis method measuring gallium in rafifinal.
Background technology
Rafifinal is silvery white in color, any surface finish, has clear crystallization line, does not contain field trash.Rafifinal has low change
The performances such as shape drag, high conductivity and good plasticity, be applied primarily to scientific research, electronics industry, chemical industry and
Manufacture high purity alloys, laser material and some other specific uses.With to the further understanding of rafifinal performance and exploitation, height
The application prospect of fine aluminium is more and more wide.Currently, to the analysis of gallium in rafifinal, there are no examination criteria methods both at home and abroad, can look into
To the method about gallium be mostly extraction and separation rhodamine B photometry, butyl rhodamine b spectrophotometry, sampling Graphite Furnace Atomic is inhaled
Receipts method etc., these method operating procedures are more, and labor intensity is big, take tediously long, are unfavorable for quickly measuring；The inductive coupling etc. found
Gas ions mass spectrography, inductively coupled plasma spectrometry method are directed to the inspection of gallium element in steel and alloy, precious metal alloys respectively
It surveys, it is widely different with high-purity aluminum material, if it needs to carry out a large number of experiments verification using the above method, thus it is existing from the aspect of two
There is method not to be suitable for the analysis needs of gallium in rafifinal.
Invention content
The purpose of the present invention is：It proposes that a kind of analytical element content lower limit is low, range is wide, can accurately carry out gallium analysis
Measure the analysis method of gallium element in rafifinal.
The technical scheme is that：Using inductively coupled plasma atomic emission spectrometer, the operating condition of instrument
And analytical line is as follows：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：
Cooling gas flow：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analysis
110~190rpm of pump speed；It can be seen that the time of integration：2~10s；
(1) reagent used in continuous mode is as follows：
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；Weigh 0.5000g pure iron, purity ＞ 99.99%), it is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and moves into 1000mL volumetric flasks, is diluted with water to after cooling
Scale shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
It is found out in the spectral line library of instrument and interferes relatively small, the relatively high 6-7 gallium analysis spectral line of the intensity of spectral line, the single solution of series is being composed
Spectrogram scanning, superposition are carried out on line, therefrom choose minimum point of 1 the intensity of spectral line height, aluminium base element of volume and co-existing element interference
Line is analysed as separated time spectral line；
(4) rafifinal solubility test
0.50g three parts of samples of analysis are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid are separately added into
(1.1) it is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2), 2.00mL Y Int Stds solution (1.24) and 20.0mL aluminium base liquid solutions are added in bottle
(1.23), then in first to the 6th volumetric flask respectively it is accurate be added 0.00mL, 0.50mL, 1.00mL, 2.00mL,
3.00mL and 5.00mL galliums standard solution (1.8), is diluted with water to scale, shakes up；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；It moves into and is accurately added
In the 50mL volumetric flasks of 2.00mL Y Int Stds solution (1.24), it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) b；To be not added with gallium standard
Solution is a little low mark solution, other each points can be according to sample content range as high standard solution；It is required that high standard solution point must
Gallium element analyst coverage in sample must be covered；
(7.4) concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line, using yttrium as internal standard element, instrument is standardized using low mark solution and high standard solution successively, so
Afterwards, the concentration for measuring gallium in sample solution, obtains the percentage composition of gallium.
It prepares low, high standard solution or using the close standard sample of chemical composition, matches after being handled according to (7.1)~(7.3)
Required low, high standard solution or standard sample solution is made.
The method have the advantages that：
1) inductively coupled plasma atomic emission spectrometer (ICP-AES) analysis has accurate, quick, multielement simultaneously
The characteristics of analysis, is widely used in the fields such as geology, metallurgy, machine-building, environmental protection, biomedicine, food, has good
Detection limit and analytical precision, Matrix effects are small, and linear dynamic range is wide, and analysis worker can be configured to primary standard substance
The advantages that a series of standard and sample pretreating easy (than wet chemical analysis).The means that gallium element measures usually have ratio
Color method, inductively coupled plasma atomic emission spectrometry, inductively coupled plasma atomic emissions mass spectrography) sampling Graphite Furnace Atomic
Absorption process etc..Corresponding analysis method can be found for the different-alloy trade mark, it is domestic at present about the analysis of gallium in rafifinal
The outer method that nothing accurately analyzes the element, is substantially and applies mechanically Ni-based, iron-base superalloy, noble metal or other alloy sides
The shortcomings of method, there are dissolved samples for using method not exclusively, the selection of analytical line is uncertain etc. causes analytical cycle longer.
2) one of the advantages of sample treatment technology is the invention, the present invention is using addition 10mL~20mL hydrochloric acid (1.4), electricity
Low-grade fever to sample dissolves on hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2) is removed from electric hot plate, heating is molten by rafifinal
Solution is complete.The present invention dissolves rafifinal with dilute hydrochloric acid, and hydrochloric acid in sample is not dissolved aliquot (few) with nitric acid
Dissolving is complete；
3) by carrying out interference experiment, it is determined that optimized analysis spectral line improves the accuracy of measurement；
4) method measurement range is wide, and it is 0.0005% to measure offline, and it is 0.005% to measure the upper limit；
5) measurement method for using internal standard element, can make measurement result more stable, be suitable for arbitrary content elemental analysis；
6) it uses synchronization process sample and prepares high and low mark solution and measure gallium element, the system reduced in analytic process is missed
Difference, analytical error is minimum under such situation, and method is reproducible；
7) Determination of Trace Gallium elemental analysis, preferable analysis result can be obtained by directly measuring；
8) hydrochloric acid, nitron use MOS grades or sub-boiling distillation reagent, are conducive to the measurement of trace and Minor element；
9) addition 0.0005%~0.005%, the rate of recovery 90.0%~105.0%, relative standard deviation is less than
9.5%, the rate of recovery, precision are preferable；
10) it is compared by the analysis of standard sample, method reinspection and with other unit analysis result and shows made fixed point
The accuracy of analysis method is good, and method is stablized, and the requirement of trace analysis is complied fully with.
11) the application method measures quick, easy to operate, has saved a large amount of man power and materials.
Specific implementation mode
Embodiment one
Gallium content in rafifinal is measured, using inductively coupled plasma atomic emission spectrometer, the operating condition of instrument
And analytical line is as follows：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：
Cooling gas flow：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analysis
110~190rpm of pump speed；It can be seen that the time of integration：2~10s；
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；0.5000g pure iron is weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to quarter
Degree, shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
On instrument by the single solution of series 294.364nm, 417.206nm, 287.424nm, 403.298nm, 209.134nm,
Spectrogram scanning, superposition are carried out on 405.007nm spectral lines, therefrom choose 294.364nm as separated time spectral line；
(4) rafifinal solubility test
Three parts of 0.50g samples are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；Studies have shown that measurement result relative standard is inclined when being not added with Y Int Std solution and 1.00mL~5.00mL Y Int Std solution is added
Difference is smaller, measures and stablizes；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2), 2.00mL Y Int Stds solution (1.24) and 20.0mL aluminium base liquid solutions are added in bottle
(1.23), then in first to the 6th volumetric flask respectively it is accurate be added 0.00mL, 0.50mL, 1.00mL, 2.00mL,
3.00mL and 5.00mL galliums standard solution (1.8), is diluted with water to scale, shakes up；
Studies have shown that having weaker background interference, calibration bent the measurement of gallium containing aluminium element in aluminum substrate working curve
Line should use aluminum substrate to match；Working curve is in a linear relationship, related coefficient 0.999927；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；It moves into and is accurately added
In the 50mL volumetric flasks of 2.00mL Y Int Stds solution (1.24), it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) b；To be not added with gallium standard
Solution is a little low mark solution, other each points can be according to sample content range as high standard solution；It is required that high standard solution point must
Gallium element analyst coverage in sample must be covered；
(7.4), the concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line 294.364nm, using yttrium as internal standard element, instrument is carried out using low mark solution and high standard solution successively
Then standardization measures the concentration of gallium in sample solution, the percentage composition for obtaining gallium is 0.0051%.
Embodiment two
Measure gallium content in rafifinal, using inductive coupling plasma emission spectrograph, the operating condition of instrument and point
It is as follows to analyse line：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：It is cooling
Throughput：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analyze pump speed
110~190rpm；It can be seen that the time of integration：2~10s；
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；0.5000g pure iron is weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to quarter
Degree, shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
On instrument by the single solution of series 294.364nm, 417.206nm, 287.424nm, 403.298nm, 209.134nm,
Spectrogram scanning, superposition are carried out on 405.007nm spectral lines, therefrom choose 407.206nm as separated time spectral line；
(4) rafifinal solubility test
Three parts of 0.50g samples are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；Studies have shown that measurement result relative standard is inclined when being not added with Y Int Std solution and 1.00mL~5.00mL Y Int Std solution is added
Difference is smaller, measures and stablizes；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 20.0mL aluminium bases liquid solution (1.23) are added in bottle, then at first to the 6th
It is accurate respectively in volumetric flask that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution is added
(1.8), it is diluted with water to scale, is shaken up；
Studies have shown that having weaker background interference, calibration bent the measurement of gallium containing aluminium element in aluminum substrate working curve
Line should use aluminum substrate to match；Working curve is in a linear relationship, related coefficient 0.999892；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Move into 50mL volumetric flasks
In, it is diluted with water to scale, is shaken up；
(7.3), calibration solution is prepared；
Point in working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) b；To be not added with gallium standard
Solution is a little low mark solution, other each points can be according to sample content range as high standard solution；It is required that high standard solution point must
Gallium element analyst coverage in sample must be covered；
(7.4) concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line 417.206nm, instrument is standardized using low mark solution and high standard solution successively, then, surveys
The concentration for measuring gallium in sample solution, the percentage composition for obtaining gallium are 0.00047%.
Embodiment three
Measure gallium content in rafifinal, using inductive coupling plasma emission spectrograph, the operating condition of instrument and point
It is as follows to analyse line：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：It is cooling
Throughput：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analyze pump speed
110~190rpm；It can be seen that the time of integration：2~10s；
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；0.5000g pure iron is weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to quarter
Degree, shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
On instrument by the single solution of series 294.364nm, 417.206nm, 287.424nm, 403.298nm, 209.134nm,
Spectrogram scanning, superposition are carried out on 405.007nm spectral lines, therefrom choose 287.424nm as separated time spectral line；
(4) rafifinal solubility test
Three parts of 0.50g samples are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；Studies have shown that measurement result relative standard is inclined when being not added with Y Int Std solution and 1.00mL~5.00mL Y Int Std solution is added
Difference is smaller, measures and stablizes；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 20.0mL aluminium bases liquid solution (1.23) are added in bottle, then at first to the 6th
It is accurate respectively in volumetric flask that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution is added
(1.8), it is diluted with water to scale, is shaken up；
C. standard sample prepares working curve containing aluminum substrate：Using the close rafifinal standard sample of chemical composition, according to
(7.1)~(7.3) it is configured to required low, high standard solution after handling, suitable gallium mark is added in standard sample solution when necessary
Quasi- solution (1.8), the working curve of preparation are shown in Table 1.
1 standard sample preparation work curve of table
| Working curve point | E5 (low mark solution) | E6 | E21 | E2 | E34 |
| Percentage composition % | 0.00021 | 0.00067 | 0.0026 | 0.00045 | 0.00056 |
Studies have shown that prepare aluminium element in working curve containing aluminum substrate containing standard sample has the weaker back of the body to the measurement of gallium
Scape interferes, and calibration curve should use aluminum substrate to match；Working curve is in a linear relationship, related coefficient 0.999902；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Move into 50mL volumetric flasks
In, it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in standard sample working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) c；With gallium
Percentage composition it is minimum a little be low mark solution (E5), other each points can be according to sample content range as high standard solution；It is required that
High standard solution point must cover gallium element analyst coverage in sample；
(7.4) concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line 287.424nm, instrument is standardized using low mark solution and high standard solution successively, then, surveys
The concentration for measuring gallium in sample solution, the percentage composition for obtaining gallium are 0.0017%.
Example IV
Gallium content in rafifinal is measured, using inductively coupled plasma atomic emission spectrometer, the operating condition of instrument
And analytical line is as follows：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：
Cooling gas flow：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analysis
110~190rpm of pump speed；It can be seen that the time of integration：2~10s；
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；0.5000g pure iron is weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to quarter
Degree, shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
On instrument by the single solution of series 294.364nm, 417.206nm, 287.424nm, 403.298nm, 209.134nm,
Spectrogram scanning, superposition are carried out on 405.007nm spectral lines, therefrom choose 403.298nm as separated time spectral line；
(4) rafifinal solubility test
Three parts of 0.50g samples are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；Studies have shown that measurement result relative standard is inclined when being not added with Y Int Std solution and 1.00mL~5.00mL Y Int Std solution is added
Difference is smaller, measures and stablizes；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 20.0mL aluminium bases liquid solution (1.23) are added in bottle, then at first to the 6th
It is accurate respectively in volumetric flask that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution is added
(1.8), it is diluted with water to scale, is shaken up；
C. standard sample prepares working curve containing aluminum substrate：Using the close rafifinal standard sample of chemical composition, according to
(7.1)~(7.3) it is configured to required low, high standard solution after handling, it is molten that suitable gallium standard is added in standard sample solution
Liquid (1.8), the working curve of preparation are shown in Table 2.
2 standard sample preparation work curve of table
Studies have shown that prepare aluminium element in working curve containing aluminum substrate containing standard sample has the weaker back of the body to the measurement of gallium
Scape interferes, and calibration curve should use aluminum substrate to match；Working curve is in a linear relationship, related coefficient 0.999934；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Move into 50mL volumetric flasks
In, it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in standard sample working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) c；With gallium
Percentage composition it is minimum a little be low mark solution (E5), other each points can be according to sample content range as high standard solution；It is required that
High standard solution point must cover gallium element analyst coverage in sample；
(7.4) concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line 403.298nm, instrument is standardized using low mark solution and high standard solution successively, then, surveys
The concentration for measuring gallium in sample solution, the percentage composition for obtaining gallium are 0.0034%.
Embodiment five
Gallium content in rafifinal is measured, using inductively coupled plasma atomic emission spectrometer, the operating condition of instrument
And analytical line is as follows：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Reflection power：＜ 15W；Argon flow amount：
Cooling gas flow：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Rinse 110~190rpm of pump speed；Analysis
110~190rpm of pump speed；It can be seen that the time of integration：2~10s；
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL capacity is moved into after cooling
In bottle, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.9) iron standard solution：0.50mg/mL；0.5000g pure iron is weighed, purity ＞ 99.99% is placed in 200mL beakers
In, 20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to quarter
Degree, shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, 500mL volumetric flasks are placed in
In, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, mixing；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL burnings
In cup, 20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, be diluted with water to quarter
Degree, shakes up；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, 500mL capacity is placed in
In bottle, 10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL burnings
In cup, 40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, dissolves by heating salt, it is cold
But it moves into 1000mL volumetric flasks afterwards, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, 500mL capacity is placed in
In bottle, 20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, is used
Water dissolution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, 500mL capacity is placed in
In bottle, 25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers,
It is blown into secondary water 10mL, 10mL nitric acid (1.2) is added, is heated to manganese and is completely dissolved, moves into 1000mL volumetric flasks, uses after cooling
Water is diluted to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, 500mL capacity is placed in
In bottle, 10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers,
50mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：Prepare the single solution of series, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-baseds
Liquid solution (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions
(1.16), 2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL
Yttrium standard solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL gallium standard solution
(1.8) and 5.00mL galliums standard solution (1.8) is respectively in 50mL volumetric flasks, in inductively coupled plasma atomic emission spectrum
On instrument by the single solution of series 294.364nm, 417.206nm, 287.424nm, 403.298nm, 209.134nm,
Spectrogram scanning, superposition are carried out on 250.017nm spectral lines, therefrom choose 250.017nm as separated time spectral line；
(4) rafifinal solubility test
Three parts of 0.50g samples are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) in electricity
It is heated on stove, rafifinal does not almost dissolve；
Weigh three parts of 0.50g samples, be separately added into 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and
5mL nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4), electric heating is added
Low-grade fever to sample dissolves on plate；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away nitrogen
Oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；Studies have shown that measurement result relative standard is inclined when being not added with Y Int Std solution and 1.00mL~5.00mL Y Int Std solution is added
Difference is smaller, measures and stablizes；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24) is added, then in first to the 6th capacity
It is accurate respectively in bottle that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) is added, it uses
Water is diluted to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th capacity
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 20.0mL aluminium bases liquid solution (1.23) are added in bottle, then at first to the 6th
It is accurate respectively in volumetric flask that 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution is added
(1.8), it is diluted with water to scale, is shaken up；
C. standard sample prepares working curve containing aluminum substrate：Using the close rafifinal standard sample of chemical composition, according to
(7.1)~(7.3) it is configured to required low, high standard solution after handling, it is molten that suitable gallium standard is added in standard sample solution
Liquid (1.8), the working curve of preparation are shown in Table 2.
2 standard sample preparation work curve of table
Studies have shown that prepare aluminium element in working curve containing aluminum substrate containing standard sample has the weaker back of the body to the measurement of gallium
Scape interferes, and calibration curve should use aluminum substrate to match；Working curve is in a linear relationship, related coefficient 0.999934；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL is added
Hydrochloric acid (1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electricity are removed from electric hot plate
Low-grade fever on hot plate drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Move into 50mL volumetric flasks
In, it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in standard sample working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) c；With gallium
Percentage composition it is minimum a little be low mark solution (E5), other each points can be according to sample content range as high standard solution；It is required that
High standard solution point must cover gallium element analyst coverage in sample；
(7.4) concentration of gallium in sample solution is measured；The work selected by inductively coupled plasma atomic emission spectrometer
Make condition and analysis spectral line 250.017nm, instrument is standardized using low mark solution and high standard solution successively, then, surveys
The concentration for measuring gallium in sample solution, the percentage composition for obtaining gallium are 0.0044%.
Claims (2)
1. a kind of analysis method measuring gallium element in rafifinal, it is characterised in that：It is sent out using inductively coupled plasma atom
Spectrometer is penetrated, the operating condition and analytical line of instrument are as follows：Higher frequency：40.68MHz；Incident power：0.95~1.5kW；Instead
Penetrate power：＜ 15W；Argon flow amount：Cooling gas flow：13~20L/min；Secondary air amount：0.2~1.0L/min；Pump speed：Punching
Wash 110~190rpm of pump speed；Analyze 110~190rpm of pump speed；It can be seen that the time of integration：2~10s；
(1) reagent used in continuous mode is as follows：
(1.1) hydrochloric acid, ρ 1.19g/mL；MOS grades or sub-boiling distillation reagent；
(1.2) nitric acid, ρ 1.42g/mL；MOS grades or sub-boiling distillation reagent；
(1.3) sulfuric acid, ρ 1.84g/mL；High purity reagent or top pure grade；
(1.4) hydrochloric acid, 1+1；
(1.5) sulfuric acid, 1+1；
(1.6) sodium hydroxide solution, 100g/L；
(1.7) gallium standard solution：0.50mg/mL；The pure galliums of 0.5000g are weighed, purity ＞ 99.99% is placed in 200mL beakers,
15mL hydrochloric acid (1.4) is added, is heated to gallium and is completely dissolved, adds 10 drop nitric acid (1.2), 1000mL volumetric flasks is moved into after cooling
In, it is diluted with water to scale, is shaken up；
(1.8) gallium standard solution：0.005mg/mL；5.00mL galliums standard solution (1.7) is pipetted, is placed in 500mL volumetric flasks, is mended
Add 10mL hydrochloric acid (1.4), is diluted with water to scale, shakes up；
(1.9) iron standard solution：0.50mg/mL；Weigh 0.5000g pure iron, purity ＞ 99.99%), it is placed in 200mL beakers,
20mL hydrochloric acid (1.4) is added, low-temperature heat is complete to dissolving, and is moved into 1000mL volumetric flasks after cooling, is diluted with water to scale,
It shakes up；
(1.10) iron standard solution：0.005mg/mL；5.00mL iron standard solution (1.9) is pipetted, is placed in 500mL volumetric flasks,
10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.11) copper standard solution：0.50mg/mL；0.5000g fine copper is weighed, purity ＞ 99.99% is placed in 200mL beakers,
20mL hydrochloric acid (1.4) is added, is heated to copper and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, is diluted with water to scale, mixed
It is even；
(1.12) copper standard solution：0.005mg/mL；5.00mL copper standard solution (1.11) is pipetted, is placed in 500mL volumetric flasks,
10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.13) magnesium standard solution：0.50mg/mL；The pure magnesium of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL beakers,
20mL hydrochloric acid (1.4) is added, is heated to magnesium and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, is diluted with water to scale, mixed
It is even；
(1.14) magnesium standard solution：0.005mg/mL；5.00mL magnesium standard solutions (1.13) are pipetted, are placed in 500mL volumetric flasks,
10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.15) Zinc standard solution：0.50mg/mL；The pure zinc of 0.5000g is weighed, purity ＞ 99.99% is placed in 200mL beakers,
20mL hydrochloric acid (1.4) is added, is heated to zinc and is completely dissolved, is moved into 1000mL volumetric flasks after cooling, is diluted with water to scale, shakes
It is even；
(1.16) Zinc standard solution：0.005mg/mL；5.00mL Zinc standard solutions (1.13) are pipetted, are placed in 500mL volumetric flasks,
10mL hydrochloric acid (1.4) is added, scale is diluted with water to, shakes up；
(1.17) titanium standard solution：0.50mg/mL；The pure titaniums of 0.5000g are weighed, purity ＞ 99.99% is placed in 300mL beakers,
40mL sulfuric acid (1.5) is added, is heated to titanium and is completely dissolved, 5 drop nitric acid (1.2) are added dropwise, blow water, salt is dissolved by heating, after cooling
It moves into 1000mL volumetric flasks, is diluted with water to scale, shakes up；
(1.18) titanium standard solution：0.005mg/mL；5.00mL titaniums standard solution (1.17) is pipetted, is placed in 500mL volumetric flasks,
20mL sulfuric acid (1.5) is added, scale is diluted with water to, shakes up；
(1.19) silicon standard solution 0.5mg/mL；1.012g sodium metasilicate is weighed, is set in 100mL polytetrafluoroethylene beakers, use is water-soluble
Solution；2mL sodium hydroxides (1.6) are added, moves into 200mL plastics volumetric flasks, is diluted with water to scale, mixing；
(1.20) silicon standard solution：0.005mg/mL；5.00mL silicon standard solution (1.20) is pipetted, is placed in 500mL volumetric flasks,
25mL hydrochloric acid (1.1) is added, scale is diluted with water to, shakes up；
(1.21) manganese standard solution 0.50mg/mL；Weigh 0.5000g；99.99% pure manganese of ＞, is placed in 200mL beakers, is blown into
Secondary water 10mL is added 10mL nitric acid (1.2), is heated to manganese and is completely dissolved, and is moved into 1000mL volumetric flasks after cooling, dilute with water
It releases to scale, mixing；
(1.22) manganese standard solution：0.005mg/mL；5.00mL manganese standard solution (1.21) is pipetted, is placed in 500mL volumetric flasks,
10mL nitric acid (1.2) is added, scale is diluted with water to, shakes up；
(1.23) aluminium base liquid solution 25.0mg/mL；5.000g is weighed, 99.999% fine aluminiums of ＞ are placed in 500mL beakers, are added
50mL hydrochloric acid (1.4), low-temperature heat is complete to dissolving, and is moved into 200mL volumetric flasks after cooling, is diluted with water to scale, shakes up；
(1.24) Y Int Std solution, 0.2mg/mL；0.127g is weighed, 99.95% yttrium oxides of ＞ are placed in 250mL beakers, are added
20mL hydrochloric acid (1.4), low-temperature heat is complete to dissolving, and is moved into 500mL volumetric flasks after cooling, is diluted with water to scale, shakes up；
(2) sampling and sample preparation；The sample of analysis is sampled according to the requirement of HB/Z 205 and sample preparation；
(3) element analysis spectrum line selects：The single solution of series is prepared, 20.0mL aluminium bases liquid solution (1.23), 5.0mL iron-based bodies are molten
Liquid (1.10), 5.0mL copper standard solution (1.12), 5.0mL magnesium standard solutions (1.14), 5.0mL Zinc standard solutions (1.16),
2.00mL standard solution (1.18), 5.0mL silicon standard solution (1.20), 5.0mL manganese standard solution (1.22), 5.0mL yttrium standards
Solution (1.24), 20mL hydrochloric acid (1.4), 8mL nitric acid (1.2), 20mL sulfuric acid (1.5), 0.50mL galliums standard solution (1.8) and
5.00mL galliums standard solution (1.8) is respectively placed in 50mL volumetric flasks, and interference is found out in the spectral line library of Atomic Emission Spectrometer AES
The single solution of series on spectral line is carried out spectrogram scanning, folded by relatively small, the relatively high 6-7 gallium analysis spectral line of the intensity of spectral line
Add, therefrom chooses the analytical line of 1 the intensity of spectral line height, aluminium base element of volume and co-existing element interference minimum as separated time spectral line；
(4) rafifinal solubility test
0.50g three parts of samples of analysis are weighed, 5mL hydrochloric acid (1.1), 10mL hydrochloric acid (1.1), 15mL hydrochloric acid (1.1) is separately added into and exists
It is heated on electric furnace, rafifinal dissolving is incomplete；
Three parts of 0.50g samples are weighed, are separately added into 3mL nitric acid (1.2), 5mL nitric acid (1.2), 8mL nitric acid (1.2) on electric furnace
It is heated, rafifinal does not almost dissolve；
Three parts of 0.50g samples are weighed, 10mL hydrochloric acid (1.4) and 3mL nitric acid (1.2), 15mL hydrochloric acid (1.4) and 5mL are separately added into
Nitric acid (1.2), 20mL hydrochloric acid (1.4) and 8mL nitric acid (1.2) are heated on electric furnace, and rafifinal dissolving is complete；
(5) Y Int Std dosage is tested
Six parts of 0.50g samples are weighed, 0.0001g is accurate to and is placed in 150mL beakers, 20mL hydrochloric acid (1.4) are added, on electric hot plate
Low-grade fever to sample dissolves；It is removed from electric hot plate slightly cold, 8mL nitric acid (1.2) is added, low-grade fever on electric hot plate drives away the oxidation of nitrogen
Object, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；Immigration be not added with internal standard and accurately be added 1.00mL,
In the 50mL volumetric flasks of 2.00mL, 3.00mL, 4.00mL and 5.00mL Y Int Std solution (1.24), it is diluted with water to scale, is shaken
It is even；
(6) Matrix effects and working curve linear test
A. reagent preparation blank working curve：Six 50mL volumetric flasks are taken, are added in first to the 6th volumetric flask respectively
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2) and 2.00mL Y Int Stds solution (1.24), then in first to the 6th volumetric flask
Accurate addition 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL gallium standard solution (1.8) respectively, it is dilute with water
It releases to scale, shakes up；
B. working curve containing aluminum substrate is prepared：In addition six 50mL volumetric flasks are taken, respectively in first to the 6th volumetric flask
15mL hydrochloric acid (1.4), 5mL nitric acid (1.2), 2.00mL Y Int Stds solution (1.24) and 20.0mL aluminium base liquid solutions is added
(1.23), then in first to the 6th volumetric flask respectively it is accurate be added 0.00mL, 0.50mL, 1.00mL, 2.00mL,
3.00mL and 5.00mL galliums standard solution (1.8), is diluted with water to scale, shakes up；
(7) analytical procedure is as follows：
(7.1) sample：0.50g samples are weighed, 0.0001g is accurate to；
(7.2) sample solution is prepared：The sample of analytical procedure (7.1) is placed in 150mL beakers, 10mL~20mL hydrochloric acid is added
(1.4), low-grade fever to sample dissolves on electric hot plate；Slightly cold, addition 3mL~8mL nitric acid (1.2), electric hot plate are removed from electric hot plate
Upper low-grade fever drives away nitrogen oxide, blows water, and dissolved salts are boiled in heating；Test solution is cooled down to room temperature；It moves into and is accurately added
In the 50mL volumetric flasks of 2.00mL Y Int Stds solution (1.24), it is diluted with water to scale, is shaken up；
(7.3) calibration solution is prepared；
Point in working curve containing aluminum substrate is prepared as low mark solution and high standard solution using (6) b；To be not added with gallium standard solution
A little be low mark solution, other each points can be according to sample content range as high standard solution；It is required that high standard solution point must cover
Gallium element analyst coverage in lid sample；
(7.4) concentration of gallium in sample solution is measured；The work item selected by inductively coupled plasma atomic emission spectrometer
Part and analysis spectral line are successively standardized instrument using low mark solution and high standard solution using yttrium as internal standard element, then,
The concentration for measuring gallium in sample solution, obtains the percentage composition of gallium.
2. a kind of analysis method measuring gallium element in rafifinal according to claim 1, characterized in that prepare low, high
It marks solution or using the close standard sample of chemical composition, is configured to after being handled according to (7.1)~(7.3) required low, high
Mark solution or standard sample solution.
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