CN101660995A - Method of measuring total content of rare earth in rare earth chrome-manganese-silicon inoculant - Google Patents
Method of measuring total content of rare earth in rare earth chrome-manganese-silicon inoculant Download PDFInfo
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Abstract
The invention discloses a method of measuring the total content of rare earth in rare earth chrome-manganese-silicon inoculant, belonging to the technical field of the metal test and analysis. The specific measuring method comprises the following steps: choice of test conditions, interference elimination, test method, working curve linear relation and recovery test. By adopting the test method ofthe invention to test the recovery, the result of the test according to the three standard added values of rare earth elements shows that when the standard value is 5.22%, the test result is 5.12%, the recovery of the test is 98.08%; when the standard value is 5.10%, the test result is 5.03%, the recovery of the test is 98.63%; when the standard value is 8.66%, test result is 8.77% and the recovery of the test is 101.27%. Therefore, the recovery of the total content of rare earth in rare earth chrome-manganese-silicon inoculant measured by the method of the invention is 98-102% so as to meet the demands of daily inspection and scientific research.
Description
[technical field]
The invention belongs to the metallic test analysis technical field, relate to a kind of method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount, particularly relate to the spectrophotometry technology of rare earth-Cr-Mn silicon inoculant middle rare earth total amount.
[technical background]
Known, the rare earth-Cr-Mn silicon inoculant is a kind of novel stabilising inovulant that domestic casting industry uses, and is usually used in the casting of breeding of thin-wall high intensity foundry goods; Rare earth element in this new inoculant has extremely strong desulfurization, deoxidizing capacity, and good fade resistance energy is arranged; Can eliminate or reduce plumbous and titanium deleterious effect so in casting process, add the inovulant contain rare earth element on a small quantity to grey cast iron flake graphite form, reduced accordingly because the chromium element adds cause cold excessively separately, strengthen matrix, improve the intensity and the wearing quality of thin-section casting cylinder body, cylinder cap.Therefore the accurate mensuration of rare earth-Cr-Mn silicon inoculant middle rare earth constituent content has a very important role and meaning to casting technique.
What at present, the mensuration of trace rare-earth adopted in the iron and steel is the mensuration employing spectrophotometric method of spectrophotometric method and magnesium-rare earth middle rare earth; " relevant report of finding through inspection information has two pieces, and the mensuration of novel rare earth chromic manganese-silicon inoculant middle rare earth does not also have relevant information.Because chromium, manganese, silicon, content of rare earth are higher, handle general wet method dissolving the early stage of sample and be difficult to make decomposed sample complete, and iron matrix, chromium all are coloured ions in the sample, and colour developing liquid is all had interference, are unfavorable for the technological process in later stage in the rare earth-Cr-Mn-Si.
List of references:
1), Lu Zhonglu, symbol is peaceful, Song Chunzhi, etc. use metallurgical analysis [M]. Shenyang: Liaoning Science Press, 1990.P-219;
2), Long Rucheng, Meng Ping, Gan Xinpei. chlorophosphonazo III spectrophotometry magnesium-rare earth middle rare earth total amount. " metallurgical analysis " [J] .2004 first phase .p-43.
[summary of the invention]
In order to overcome the deficiency of existing technology, the invention provides a kind of method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount; The method of mensuration rare earth-Cr-Mn silicon inoculant middle rare earth total amount of the present invention adopts the alkali fusion sample, under suitable acidity, utilize chlorophosphonazo III to be developer, oxalic acid is screening agent, and use the colour developing liquid that sodium hexametaphosphate solution fades to make reference liquid, the spectrophotometric direct method is measured rare earth-Cr-Mn silicon inoculant middle rare earth total amount; The data that the present invention draws by described method have highly sensitive, good stability, measurement result increases substantially than potassium fluosilicate precipitate and separate volumetric determination rare earth relative accuracy, operation is also corresponding fast convenient, can satisfy the requirement of the total quantitative determination of novel rare inovulant soil chromium manganese silicon middle rare earth.
In order to realize the foregoing invention purpose, the present invention adopts following technical scheme:
A kind of method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount: described method is the spectrophotometric method method of inspection of rare earth-Cr-Mn silicon inoculant middle rare earth total amount, and concrete check comprises selection, interference eliminated, test method, the working curve linear relationship of test condition, the checking procedure of the recovery;
Reagent is: sodium peroxide " solid "; Chlorophosphonazo III: 4gL
-1It is pure that described reagent is analysis;
Use therein instrument is a 723N type spectrophotometer " Shanghai Precision Scientific Apparatus Co., Ltd ";
Concrete steps are as follows:
One, experiment condition:
Handle the early stage of A, sample;
Need to prove that it is key of the present invention that sample is handled,, dissolve with general sour wet method and be difficult to make sample to dissolve fully because chromium in the rare earth-Cr-Mn-Si, manganese, silicone content are higher; Select for use the method for sodium peroxide high-temperature fusion to handle sample among the present invention, and then use sour acidified sample; Take by weighing the 0.5000g sample, select for use the sodium peroxide of 2～8g to carry out the happy and harmonious test of sample, determine that the used sodium peroxide amount of fusion sample is 4～8g; The acid that test solution after the acidifying fusion is commonly used has the acid mixture of hydrochloric acid, sulfuric acid or nitric acid or described several acid, needs according to the follow-up test part, preferred red fuming nitric acid (RFNA) acidifying, selecting the red fuming nitric acid (RFNA) amount for use is that 20～70mL carries out the acidifying experiment to fusing sample, and wherein can reach complete acidifying and don't influence measuring for acid of subsequent experimental step is 30～60mL;
The temperature and time control of B, fusing sample;
With sodium peroxide fusion sample in nickel crucible, should make the complete fusion of sample, consider that again nickel crucible is not penetrated, select the melt temperature and the time that suit; Take by weighing the 0.5000g sample, put into the nickel crucible that fills 4～8g sodium peroxide, with 600～800 ℃ temperature fusing sample, wherein the suitable melt temperature of Que Dinging is 650～750 ℃; Be that 10～30min tests to the melting time simultaneously, determine that the suitable melting time is 15～30min;
C, developer, screening agent reagent dosage;
Developer addition: respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 10 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL respectively, oxalic acid solution 0.5～2.5mL; , in 10 50mL volumetric flasks, add the chlorophosphonazo III solution of 0～10mL successively, be diluted to scale and shake up, place 15min after, in 680nm wavelength place, carry out light absorption value mensuration with the 2cm cuvette; Chlorophosphonazo III addition hour colour developing not exclusively increases the amount of chlorophosphonazo III, and absorbance descends on the contrary; Therefore, the developer optimal addn is 4～7mL;
The addition of oxalic acid: in order to keep acidity, can eliminate the interference example again, and not influence the rare earth chromogenic reaction, the oxalic acid addition just must have certain scope; Respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 9 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL, add 0,0.5,1,1.5,2,2.5,3,3.5 successively respectively, the 4mL oxalic acid solution, chlorophosphonazo III solution is 4～7mL, be diluted to scale and shake up, behind the placement 15min, in 680nm wavelength place, carry out light absorption value with the 2cm cuvette and measure, 50gL is determined in test
-1The suitable addition of oxalic acid solution is 0.5～2.5mL;
The influence of D, acidity;
Behind nitric acid and the hydrofluoric acid treatment test solution, solution has certain acidity; When measuring rare earth, color acidity should be controlled in the slightly acidic solution of pH2.5～3.5, and rare earth ion and chlorophosphonazo III form 1: 1 the stable complex compound of bluish violet; The present invention adopts sulfuric acid further to adjust acidity, respectively gets the rare earth alloy standard specimen solution 5mL that handles well and places 8 50mL volumetric flasks respectively, adds 0,0.5,1,1.5,2,2.5,3 successively respectively, 3.5mL sulfuric acid 0.9molL
-1, add 50gL
-1Oxalic acid solution is 0.5～2.5mL, and chlorophosphonazo III solution is 4～7mL, is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, carries out light absorption value with the 2cm cuvette and measures; Acidity is too big or too little, and absorbance all diminishes; Through overtesting sulfuric acid 0.9molL
-1Addition be 1.5～2.5mL;
Two, the elimination of coexistence elements interference;
Main secondary element is rare earth, chromium, manganese, silicon, iron in the rare earth-Cr-Mn silicon inoculant; A large amount of iron, manganese, chromium adopt the interference of measuring rare earth:
(1) adds the interference that ferric ion and manganese ion are sheltered in the oxalic acid solution complexing;
(2) get a certain amount of colour developing liquid and add sodium hexametaphosphate solution, the solution after the color of elimination rare earth and chlorophosphonazo III complex ion is made reference liquid, to eliminate the interference of coloured ions such as chromium ion;
Three, test method;
Take by weighing sample 0.25000g and place the nickel crucible that fills 4～8g sodium peroxide, stir, put into 650～750 ℃ of high temperature furnace fusion 15～30min, take out cooling and put into the 400mL polytetrafluoroethylene beaker, add the leaching of 100mL hot water and melt piece, heated and boiled 2min slowly adds red fuming nitric acid (RFNA) 30～60mL souring soln, heated and boiled, it is droplet limpid fully to solution to drip the sodium nitrite solution number, boils 2min, changes in the 250mL volumetric flask after taking off cooling, water is settled to scale, shakes up to be measured;
Draw above-mentioned mother liquor 50mL and place the 250mL plastic beaker, add hydrofluorite 2mL, catch up with most nitrogen dioxide after, add 100mL 5% BAS, change in the 500mL volumetric flask after placing 10min, water is settled to scale, shakes up;
Draw above-mentioned solution 5mL and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
-1Oxalic acid solution, 4～7mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
-12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion;
Four, working curve linear relationship;
With a content of rare earth is that 20.09% high rare earth alloy standard specimen " is numbered machine word 57 ", by " three, test method " step operation, is with reagent blank simultaneously; Divide and to get that different these standard specimens of amount are 0,0.5,1.0,1.5,2.0,2.5mL makes curve, by " three, test method " step operation; At maximum absorption wavelength 680nm, concentration 50 μ g/50mL are with the interior Lambert-Beer's law that meets, linear equation: A=0.1530X-0.0099, linearly dependent coefficient r=0.9996;
Five, the recovery;
Standard content with adding rare earth element adopts the test method time-and-motion study recovery of the present invention, and three standard adding values of measurement result rare earth element are measured, and standard value is 5.22%, and measurement result is 5.12%, and measuring the recovery is 98.08%; Standard value is 5.10%, and measurement result is 5.03%, and measuring the recovery is 98.63%; Standard value is 8.66%, and measurement result is 8.77%, and measuring the recovery is 101.27%;
The recovery that can draw the ree content in this method mensuration rare earth-Cr-Mn silicon inoculant can be crossed and satisfy the daily check and the requirement of scientific research between 98%～102%.
Owing to adopted technique scheme, the present invention to have following beneficial effect:
The method that is used to measure rare earth-Cr-Mn silicon inoculant middle rare earth total amount of the present invention detects rare earth-Cr-Mn silicon inoculant middle rare earth total amount by adopting spectrophotometric method.The present invention is by repeatedly check, accurate mensuration and strict control have been passed through to rare earth-Cr-Mn silicon inoculant middle rare earth total amount, effectively guaranteed the overall control of rare earth-Cr-Mn silicon inoculant middle rare earth in allowed limits, thereby guaranteed that our company's cast article uses the quality and the performance of rare earth-Cr-Mn silicon inoculant, effect is good; The present invention has highly sensitive, and the range of linearity is wide, good stability, and advantage such as easy and simple to handle, analysis result can satisfy the requirement of measuring total amount of rare earth in the rare earth-Cr-Mn silicon inoculant accurately and reliably.
[embodiment]
Disclose purpose of the present invention and be intended to protect all changes and improvements in the scope of the invention, the following examples are not concrete qualification of the present invention;
Can explain the present invention in more detail by the following examples;
A kind of method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount: described method is the spectrophotometric method method of inspection of rare earth-Cr-Mn silicon inoculant middle rare earth total amount, and concrete check comprises selection, interference eliminated, test method, the working curve linear relationship of test condition, the checking procedure of the recovery;
Reagent is: sodium peroxide " solid "; Chlorophosphonazo III: 4gL
-1It is pure that described reagent is analysis.
Use therein instrument is a 723N type spectrophotometer (Shanghai Precision Scientific Apparatus Co., Ltd);
Concrete steps are as follows:
One, experiment condition:
Handle the early stage of A, sample;
Need to prove that it is key of the present invention that sample is handled,, dissolve with general sour wet method and be difficult to make sample to dissolve fully because chromium in the rare earth-Cr-Mn-Si, manganese, silicone content are higher; Select for use the method for sodium peroxide high-temperature fusion to handle sample among the present invention, and then use sour acidified sample; Take by weighing the 0.5000g sample, select for use the sodium peroxide of 2～8g to carry out the happy and harmonious test of sample, determine that the used sodium peroxide amount of fusion sample is 4～8g; The acid that test solution after the acidifying fusion is commonly used has the acid mixture of hydrochloric acid, sulfuric acid or nitric acid or described several acid, needs according to the follow-up test part, preferred red fuming nitric acid (RFNA) acidifying, selecting the red fuming nitric acid (RFNA) amount for use is that 20～70mL carries out the acidifying experiment to fusing sample, and wherein can reach complete acidifying and don't influence measuring for acid of subsequent experimental step is 30～60mL.
The temperature and time control of B, fusing sample;
With sodium peroxide fusion sample in nickel crucible, should make the complete fusion of sample, consider that again nickel crucible is not penetrated, select the melt temperature and the time that suit; Take by weighing the 0.5000g sample, put into the nickel crucible that fills 4～8g sodium peroxide, with 600～800 ℃ temperature fusing sample, wherein the suitable melt temperature of Que Dinging is 650～750 ℃; Be that 10～30min tests to the melting time simultaneously, determine that the suitable melting time is 15～30min;
C, developer, screening agent reagent dosage;
Developer addition: respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 10 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL respectively, oxalic acid solution 0.5～2.5mL; , in 10 50mL volumetric flasks, add the chlorophosphonazo III solution of 0～10mL successively, be diluted to scale and shake up, place 15min after, in 680nm wavelength place, carry out light absorption value mensuration with the 2cm cuvette; Chlorophosphonazo III addition hour colour developing not exclusively increases the amount of chlorophosphonazo III, and absorbance descends on the contrary; Therefore, the developer optimal addn is 4～7mL;
The addition of oxalic acid: in order to keep acidity, can eliminate the interference example again, and not influence the rare earth chromogenic reaction, the oxalic acid addition just must have certain scope; Respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 9 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL, add 0,0.5,1,1.5,2,2.5,3,3.5 successively respectively, the 4mL oxalic acid solution, chlorophosphonazo III solution is 4～7mL, be diluted to scale and shake up, behind the placement 15min, in 680nm wavelength place, carry out light absorption value with the 2cm cuvette and measure, 50gL is determined in test
-1The suitable addition of oxalic acid solution is 0.5～2.5mL;
The influence of D, acidity;
Behind nitric acid and the hydrofluoric acid treatment test solution, solution has certain acidity.When measuring rare earth, color acidity should be controlled in the slightly acidic solution of pH2.5～3.5, and rare earth ion and chlorophosphonazo III form 1: 1 the stable complex compound of bluish violet.The present invention adopts sulfuric acid further to adjust acidity, respectively gets the rare earth alloy standard specimen solution 5mL that handles well and places 8 50mL volumetric flasks respectively, adds 0,0.5,1,1.5,2,2.5,3 successively respectively, 3.5mL sulfuric acid 0.9molL
-1, add 50gL
-1Oxalic acid solution is 0.5～2.5mL, and chlorophosphonazo III solution is 4～7mL, is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, carries out light absorption value with the 2cm cuvette and measures.Acidity is too big or too little, and absorbance all diminishes.Through overtesting sulfuric acid 0.9molL
-1Addition be 1.5～2.5mL.
Two, the elimination of coexistence elements interference;
Main secondary element is rare earth, chromium, manganese, silicon, iron in the rare earth-Cr-Mn silicon inoculant.A large amount of iron, manganese, chromium adopt the interference of measuring rare earth:
(1) adds the interference that ferric ion and manganese ion are sheltered in the oxalic acid solution complexing;
(2) get a certain amount of colour developing liquid and add sodium hexametaphosphate solution, the solution after the color of elimination rare earth and chlorophosphonazo III complex ion is made reference liquid, to eliminate the interference of coloured ions such as chromium ion;
Three, test method;
Take by weighing sample 0.25000g and place the nickel crucible that fills 4～8g sodium peroxide, stir, put into 650～750 ℃ of high temperature furnace fusion 15～30min, take out cooling and put into the 400mL polytetrafluoroethylene beaker, add the leaching of 100mL hot water and melt piece, heated and boiled 2min slowly adds red fuming nitric acid (RFNA) 30～60mL souring soln, heated and boiled, it is droplet limpid fully to solution to drip the sodium nitrite solution number, boils 2min, changes in the 250mL volumetric flask after taking off cooling, water is settled to scale, shakes up to be measured;
Draw above-mentioned mother liquor 50mL and place the 250mL plastic beaker, add hydrofluorite 2mL, catch up with most nitrogen dioxide after, add 100mL 5% BAS, change in the 500mL volumetric flask after placing 10min, water is settled to scale, shakes up;
Draw above-mentioned solution 5mL and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
-1Oxalic acid solution, 4～7mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
-12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion;
Four, working curve linear relationship;
With a content of rare earth is 20.09% high rare earth alloy standard specimen (being numbered machine word 57), by (three, test method) step operation, is with reagent blank simultaneously; Divide and to get that different these standard specimens of amount are 0,0.5,1.0,1.5,2.0,2.5mL makes curve, by (three, test method) step operation; At maximum absorption wavelength 680nm, concentration 50 μ g/50mL are with the interior Lambert-Beer's law that meets, linear equation: A=0.1530X-0.0099, linearly dependent coefficient r=0.9996;
Five, the recovery;
Standard content with adding rare earth element adopts the test method time-and-motion study recovery of the present invention, and measurement result sees the following form;
Following table determination of recovery rates result
The recovery that can draw the ree content in this method mensuration rare earth-Cr-Mn silicon inoculant can be crossed and satisfy the daily check and the requirement of scientific research between 98%～102%.
The method that is used to measure rare earth-Cr-Mn silicon inoculant middle rare earth total amount of the present invention, employed key instrument is: 723N spectrophotometer " Shanghai Precision Scientific Apparatus Co., Ltd ";
Reagent is: sodium peroxide " solid "; Chlorophosphonazo III: 4gL
-1It is pure that described reagent is analysis.
Embodiment one:
Handle sample by test procedure, get the rare earth-Cr-Mn-Si sample solution 5mL that handles well and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
-1Oxalic acid solution, 4mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
-12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion.
The content of the rare earth of on calibration curve, looking into conditional operation.
Embodiment two:
Handle sample by test procedure, get the rare earth-Cr-Mn-Si sample solution 5mL that handles well and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
-1Oxalic acid solution, 5mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
-12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion.
The content of the rare earth of on calibration curve, looking into conditional operation.
Embodiment three:
Handle sample by test procedure, get the rare earth-Cr-Mn-Si sample solution 5mL that handles well and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
-1Oxalic acid solution, 7mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
-12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion.
The content of the rare earth of on calibration curve, looking into conditional operation.
Embodiment four:
Take by weighing a total amount of rare earth and be 6.50% rare earth-Cr-Mn-Si sample, undertaken 7 times by the test method operation and measure, measurement result is as described in the following table:
Measurement result is more approaching, and it is as shown in the table, illustrates that the spectrophotometry of rare earth-Cr-Mn silicon inoculant middle rare earth total amount of the present invention has the advantage of structure favorable reproducibility.
Therefore, by the checking of above-mentioned embodiment, the present invention's method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount has precision height, favorable reproducibility as can be seen, the accuracy advantages of higher, be fit to total amount of rare earth be: the mensuration of 1.0～10% novel rare earth chromic manganese-silicon inoculant middle rare earth.
Claims (4)
1, a kind of method of measuring rare earth-Cr-Mn silicon inoculant middle rare earth total amount: described method is the spectrophotometric method method of inspection of rare earth-Cr-Mn silicon inoculant middle rare earth total amount, concrete check comprises selection, interference eliminated, test method, the working curve linear relationship of test condition, the checking procedure of the recovery, it is characterized in that; Concrete steps are as follows:
One, experiment condition:
Handle the early stage of A, sample;
Need to prove that it is key of the present invention that sample is handled,, dissolve with general sour wet method and be difficult to make sample to dissolve fully because chromium in the rare earth-Cr-Mn-Si, manganese, silicone content are higher; Select for use the method for sodium peroxide high-temperature fusion to handle sample among the present invention, and then use sour acidified sample; Take by weighing the 0.5000g sample, select for use the sodium peroxide of 2～8g to carry out the happy and harmonious test of sample, determine that the used sodium peroxide amount of fusion sample is 4～8g; The acid that test solution after the acidifying fusion is commonly used has the acid mixture of hydrochloric acid, sulfuric acid or nitric acid or described several acid, needs according to the follow-up test part, preferred red fuming nitric acid (RFNA) acidifying, selecting the red fuming nitric acid (RFNA) amount for use is that 20～70mL carries out the acidifying experiment to fusing sample, and wherein can reach complete acidifying and don't influence measuring for acid of subsequent experimental step is 30～60mL;
The temperature and time control of B, fusing sample;
With sodium peroxide fusion sample in nickel crucible, should make the complete fusion of sample, consider that again nickel crucible is not penetrated, select the melt temperature and the time that suit; Take by weighing the 0.5000g sample, put into the nickel crucible that fills 4～8g sodium peroxide, with 600～800 ℃ temperature fusing sample, wherein the suitable melt temperature of Que Dinging is 650～750 ℃; Be that 10～30min tests to the melting time simultaneously, determine that the suitable melting time is 15～30min;
C, developer, screening agent reagent dosage;
Developer addition: respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 10 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL respectively, oxalic acid solution 0.5～2.5mL; , in 10 50mL volumetric flasks, add the chlorophosphonazo III solution of 0～10mL successively, be diluted to scale and shake up, place 15min after, in 680nm wavelength place, carry out light absorption value mensuration with the 2cm cuvette; Chlorophosphonazo III addition hour colour developing not exclusively increases the amount of chlorophosphonazo III, and absorbance descends on the contrary; Therefore, the developer optimal addn is 4～7mL;
The addition of oxalic acid: in order to keep acidity, can eliminate the interference example again, and not influence the rare earth chromogenic reaction, the oxalic acid addition just must have certain scope; Respectively get the rare earth alloy standard specimen solution 5mL that handles well and place 9 50mL volumetric flasks respectively, add sulfuric acid solution 1.5～2.5mL, add 0,0.5,1,1.5,2,2.5,3,3.5 successively respectively, the 4mL oxalic acid solution, chlorophosphonazo III solution is 4～7mL, be diluted to scale and shake up, behind the placement 15min, in 680nm wavelength place, carry out light absorption value with the 2cm cuvette and measure, 50gL is determined in test
1The suitable addition of oxalic acid solution is 0.5～2.5mL;
The influence of D, acidity;
Behind nitric acid and the hydrofluoric acid treatment test solution, solution has certain acidity; When measuring rare earth, color acidity should be controlled in the slightly acidic solution of pH2.5～3.5, and rare earth ion and chlorophosphonazo III form 1: 1 the stable complex compound of bluish violet; The present invention adopts sulfuric acid further to adjust acidity, respectively gets the rare earth alloy standard specimen solution 5mL that handles well and places 8 50mL volumetric flasks respectively, adds 0,0.5,1,1.5,2,2.5,3 successively respectively, 3.5mL sulfuric acid 0.9molL
1, add 50gL
-1Oxalic acid solution is 0.5～2.5mL, and chlorophosphonazo III solution is 4～7mL, is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, carries out light absorption value with the 2cm cuvette and measures; Acidity is too big or too little, and absorbance all diminishes; Through overtesting sulfuric acid 0.9molL
1Addition be 1.5～2.5mL;
Two, the elimination of coexistence elements interference;
Main secondary element is rare earth, chromium, manganese, silicon, iron in the rare earth-Cr-Mn silicon inoculant; A large amount of iron, manganese, chromium adopt the interference of measuring rare earth:
(1) adds the interference that ferric ion and manganese ion are sheltered in the oxalic acid solution complexing;
(2) get a certain amount of colour developing liquid and add sodium hexametaphosphate solution, the solution after the color of elimination rare earth and chlorophosphonazo III complex ion is made reference liquid, to eliminate the interference of coloured ions such as chromium ion;
Three, test method;
Take by weighing sample 0.25000g and place the nickel crucible that fills 4～8g sodium peroxide, stir, put into 650～750 ℃ of high temperature furnace fusion 15～30min, take out cooling and put into the 400mL polytetrafluoroethylene beaker, add the leaching of 100mL hot water and melt piece, heated and boiled 2min slowly adds red fuming nitric acid (RFNA) 30～60mL souring soln, heated and boiled, it is droplet limpid fully to solution to drip the sodium nitrite solution number, boils 2min, changes in the 250mL volumetric flask after taking off cooling, water is settled to scale, shakes up to be measured;
Draw above-mentioned mother liquor 50mL and place the 250mL plastic beaker, add hydrofluorite 2mL, catch up with most nitrogen dioxide after, add 100mL 5% BAS, change in the 500mL volumetric flask after placing 10min, water is settled to scale, shakes up;
Draw above-mentioned solution 5mL and place the 50mL volumetric flask, add 1.5～2.5mL 0.9molL
-1Sulfuric acid solution adds 0.5～2.5mL 50gL
1Oxalic acid solution, 4～7mL chlorophosphonazo III solution is diluted to scale and shakes up, and behind the placement 15min, in 680nm wavelength place, the 2cm cuvette is got part colour developing liquid and is added sodium hexametaphosphate 50gL
12, carry out colorimetric as reference after taking off the color of rare earth and chlorophosphonazo III complex ion;
Four, working curve linear relationship;
With a content of rare earth is that 20.09% high rare earth alloy standard specimen " is numbered machine word 57 ", by " three, test method " step operation, is with reagent blank simultaneously; Divide and to get that different these standard specimens of amount are 0,0.5,1.0,1.5,2.0,2.5mL makes curve, by " three, test method " step operation; At maximum absorption wavelength 680nm, concentration 50 μ g/50mL are with the interior Lambert-Beer's law that meets, linear equation: A=0.1530X-0.0099, linearly dependent coefficient r=0.9996;
Five, the recovery;
Standard content with adding rare earth element adopts the test method time-and-motion study recovery of the present invention, and three standard adding values of measurement result rare earth element are measured, and standard value is 5.22%, and measurement result is 5.12%, and measuring the recovery is 98.08%; Standard value is 5.10%, and measurement result is 5.03%, and measuring the recovery is 98.63%; Standard value is 8.66%, and measurement result is 8.77%, and measuring the recovery is 101.27%;
The recovery that can draw the ree content in this method mensuration rare earth-Cr-Mn silicon inoculant can be crossed and satisfy the daily check and the requirement of scientific research between 98%～102%.
2, the method for mensuration rare earth-Cr-Mn silicon inoculant middle rare earth total amount according to claim 1 is characterized in that; Reagent is: sodium peroxide " solid "; Chlorophosphonazo III: 4gL
-1It is pure that described reagent is analysis.
3, the method for mensuration rare earth-Cr-Mn silicon inoculant middle rare earth total amount according to claim 1 is characterized in that; Use therein instrument is a 723N type spectrophotometer.
4, the method for mensuration rare earth-Cr-Mn silicon inoculant middle rare earth total amount according to claim 3 is characterized in that; Described 723N type spectrophotometric is counted Shanghai Precision Scientific Apparatus Co., Ltd and is produced.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101839861A (en) * | 2010-03-29 | 2010-09-22 | 武钢集团昆明钢铁股份有限公司 | Method for determining boron and manganese content in SYP sintering potentiating agent |
| CN102252883A (en) * | 2011-05-03 | 2011-11-23 | 武钢集团昆明钢铁股份有限公司 | Method for determining content of manganese, phosphorus, arsenic, potassium, sodium and copper in direct reduced iron |
| CN102313705A (en) * | 2010-12-07 | 2012-01-11 | 中国一拖集团有限公司 | Method for determining manganese content in hair |
| CN105548025A (en) * | 2015-12-08 | 2016-05-04 | 中国水产科学研究院南海水产研究所 | Quick detection method of carotenoid content in marine bivalve organism |
| CN110895244A (en) * | 2019-11-26 | 2020-03-20 | 天津华勘商品检验有限公司 | Method for analyzing other impurity elements in silicon-manganese-zirconium inoculant |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100352954C (en) * | 2005-04-05 | 2007-12-05 | 中国科学院长春应用化学研究所 | Technology for separating rare earth element by extraction system added with modifier |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101839861A (en) * | 2010-03-29 | 2010-09-22 | 武钢集团昆明钢铁股份有限公司 | Method for determining boron and manganese content in SYP sintering potentiating agent |
| CN101839861B (en) * | 2010-03-29 | 2011-08-31 | 武钢集团昆明钢铁股份有限公司 | Method for determining boron and manganese content in SYP sintering synergist |
| CN102313705A (en) * | 2010-12-07 | 2012-01-11 | 中国一拖集团有限公司 | Method for determining manganese content in hair |
| CN102252883A (en) * | 2011-05-03 | 2011-11-23 | 武钢集团昆明钢铁股份有限公司 | Method for determining content of manganese, phosphorus, arsenic, potassium, sodium and copper in direct reduced iron |
| CN105548025A (en) * | 2015-12-08 | 2016-05-04 | 中国水产科学研究院南海水产研究所 | Quick detection method of carotenoid content in marine bivalve organism |
| CN110895244A (en) * | 2019-11-26 | 2020-03-20 | 天津华勘商品检验有限公司 | Method for analyzing other impurity elements in silicon-manganese-zirconium inoculant |
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