CN102980886A - Measuring method of ferric content of Fe-Ce intermediate alloy - Google Patents
Measuring method of ferric content of Fe-Ce intermediate alloy Download PDFInfo
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Abstract
The invention relates to a measuring method of ferric content of a Fe-Ce intermediate alloy and belongs to the technical field of analytical chemistry. The measuring method of the ferric content of the Fe-Ce intermediate alloy is characterized in that sulfur phosphorus mixed acid resolves a sample, and the ferric content of the Fe-Ce intermediate alloy is measured by the potassium dichromate volumetric method. The measuring method of the ferric content of the Fe-Ce intermediate alloy can measure the ferric content of the Fe-Ce intermediate alloy fast and accurately.
Description
One, technical field
The invention belongs to technical field of analytical chemistry, relate to the assay method of iron content in a kind of Fe-Ce intermediate alloy.
Two, background technology
Rare earth is widely used in the different field such as metallurgy, aviation as special material, the application of rare earth in steel is still the focus of researcher research at present.Because rare earth is scarce resource, the content of iron in the Accurate Determining Fe-Ce intermediate alloy, to instruct explained hereafter, very important effect has avoided waste.Iron there is no analytical approach in the Fe-Ce intermediate alloy at present.
Three, summary of the invention
The object of the invention is to disclose the assay method of iron content in a kind of Fe-Ce intermediate alloy, but utilize the content of iron in the method Accurate Determining Fe-Ce intermediate alloy.
Come at first, by experiment to determine the span of correlation parameter and to the influence factor of assay method.
1, sample weighting amount determines
Divide another name 0.1000g, 0.2000g Fe-Ce intermediate alloy 1
#Sample is in the 300mL conical flask, adding (2+3) mixture of sulfuric phosphoric acid 20mL(2+3 mixture of sulfuric phosphoric acid is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, the results are shown in Table 1.
Table 1: definite at % of sample weighting amount
The result shows: the iron in the equal energy of the sample weighting amount of 0.1000g, the 0.2000g Accurate Determining Fe-Ce intermediate alloy, the sample weighting amount of this method is defined as 0.1000g.
2, molten sample acid determines
Divide another name 0.1000g Fe-Ce intermediate alloy 1
#, 2
#Each two parts on sample is in conical flask, the hydrochloric acid that a copy of it adds the hydrochloric acid 50mL(1+1 of 1+1 is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), the mixture of sulfuric phosphoric acid that another part adds the mixture of sulfuric phosphoric acid 20mL(2+3 of 2+3 is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly); Add the hydrochloric acid sample in low temp. electric hot plate heating for dissolving (little boiling), add mixture of sulfuric phosphoric acid sample heating for dissolving on high-temperature electric resistance furnace.Add hydrochloric acid sample continuous supplementing water in course of dissolution, take off slightly cold after the sample dissolution.The hydrochloric acid that adds respectively (1+1) hydrochloric acid 20mL(1+1 is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point.The results are shown in Table 2.
Table 2: definite at % of molten sample acid
The result shows: two kinds of nitration mixture all can dissolve Fe-Ce intermediate alloy sample, and this method is selected the mixture of sulfuric phosphoric acid dissolved samples.
3, molten sample acid amount determines
Divide another name 0.1000g Fe-Ce intermediate alloy 1
#Three parts on sample is in conical flask, add respectively (2+3) mixture of sulfuric phosphoric acid (mixture of sulfuric phosphoric acid of 2+3 is that the phosphoric acid 60mL with the sulfuric acid 40mL of ρ 1.84g/mL and ρ 1.685g/mL stirs evenly) heated sample of different amounts to dissolving fully, take off, slightly cold, the hydrochloric acid that adds respectively the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point.The results are shown in Table 3.
Table 3: definite at % of molten sample acid amount
The result shows: the mixture of sulfuric phosphoric acid addition is when 15mL～25mL, and sample is soluble and measured value stable, and the amount of the molten sample acid of this method is defined as 20mL.
4, the determining of hydrochloric acid content during the stannous chloride reduced iron
Claim 0.1000g some parts of Fe-Ce intermediate alloys 1
#In conical flask, add (2+3) mixture of sulfuric phosphoric acid (mixture of sulfuric phosphoric acid of 2+3 is that the phosphoric acid 60mL with the sulfuric acid 40mL of ρ 1.84g/mL and ρ 1.685g/mL stirs evenly) dissolved samples, the hydrochloric acid (hydrochloric acid of 1+1 is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly) that adds different amounts (1+1), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point.The results are shown in Table 4.
Table 4: definite at % of hydrochloric acid content
The result shows: during the stannous chloride reduced iron, Acidity Range is wider, and the hydrochloric acid (hydrochloric acid of 1+1 is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly) of 20mL～30mL(1+1) all can.
5, the sodium tungstate dose indicating determines
Claim 0.1000g Fe-Ce intermediate alloy 1
#Three parts on sample is in conical flask, adding (2+3) mixture of sulfuric phosphoric acid 20mL(2+3 mixture of sulfuric phosphoric acid is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly cold, heating water 50mL, the sodium tungstate that adds different amounts, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, the results are shown in Table 5.
Table 5: definite at % of sodium tungstate
The result shows: sodium tungstate is at 8 to 12 Accurate Determinings that do not affect iron.
6, the titanium trichloride amount determines
Claim 0.1000g two parts of Fe-Ce intermediate alloys 1
#Sample is in conical flask, adding (2+3) mixture of sulfuric phosphoric acid 20mL(2+3 mixture of sulfuric phosphoric acid is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly cold, heating water 50mL, add 8 sodium tungstates, portion is added dropwise to titanium trichloride and solution is stablize blue look (slightly shallow), another part is added dropwise to titanium trichloride and solution is stablize blue look (slightly dark), is titrated to blue disappearance with the potassium dichromate standard solution, adds immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, on not significantly impact of measurement result.
7, the diphenylamine sulfonic acid sodium salt amount determines
Claim 0.1000g two parts of Fe-Ce intermediate alloys 1
#Sample is in conical flask, adding (2+3) mixture of sulfuric phosphoric acid 20mL(2+3 mixture of sulfuric phosphoric acid is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, adds immediately the diphenylamine sulfonic acid sodium salt indicator of different amounts, is titrated to the potassium dichromate standard solution and stablizes purple and do not move back and be terminal point, the results are shown in Table 6.
Table 6: the determining of diphenylamine sulfonic acid sodium salt amount
The result shows: the diphenylamine sulfonic acid sodium salt indicator addition of 0.2 at % does not affect the Accurate Determining of iron in 4～6.
8, the interference experiment of coexistence elements cerium
Claim 5 parts of 0.1000g and 0.0900g high purity irons in conical flask, add respectively and be equivalent in the 0.1000g sample 2.00%, 5.00%, 10.00%, 15.00% cerium, adding respectively (2+3) mixture of sulfuric phosphoric acid 20mL(2+3 mixture of sulfuric phosphoric acid is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, inferior solution of tin 6 at% are extremely light yellow with dichloride.Take off slightly coldly, heating water 50mL adds 8 sodium tungstates, adds immediately 4 diphenylamine sulfonic acid sodium salt indicator, is titrated to the potassium dichromate standard solution and stablizes purple and do not move back and be terminal point.The results are shown in Table 7.
Table 7: coexistence elements affect at %
The result shows: 15.00 at % do not affect the Accurate Determining of iron with interior cerium in the sample.
According to the result that above-mentioned experiment obtains, the relevant parameters of determining is applied to the assay method of iron content in the Fe-Ce intermediate alloy.The technical scheme that realizes the method is such:
Sample is broken, to be ground to its granularity be 80 orders; Take by weighing sample 0.1000g in the triangular flask of 300mL, the phosphoric acid 60mL that adds (2+3) mixture of sulfuric phosphoric acid 15mL～25mL(2+3 mixture of sulfuric phosphoric acid and be the sulfuric acid 40mL of ρ 1.84g/mL and ρ 1.685g/mL stirs evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL～30mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach); Take off slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, in company with the band reagent blank.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Computing formula is:
The mass percent of W in the formula (Fe)-iron, %;
The concentration numerical value of C-potassium dichromate standard solution, mol/L;
V
0Consume the volume numerical value of potassium dichromate standard solution during-titration blank solution, mL;
Consume the volume numerical value of potassium dichromate standard solution during V-titration sample, mL;
The quality numerical value of m-sample, g;
55.85 the molal weight of-iron, g/mol.
Outstanding advantages of the present invention is: set up the assay method of iron content in a kind of Fe-Ce intermediate alloy, filled up the blank of iron content analysis field in the Fe-Ce intermediate alloy.
Four, embodiment:
The invention will be further described below in conjunction with embodiment.
The main agents preparation:
Mixture of sulfuric phosphoric acid (2+3): the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL stir evenly.
Hydrochloric acid (1+1): the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL stir evenly.
Inferior solution of tin 6 at% of dichloride: claim the inferior tin 6g of dichloride to be dissolved in the 100mL hydrochloric acid (1+1), and add several tin grains;
Sodium tungstate solution (20%): get the 25g sodium tungstate and be dissolved in the 90mL water, add phosphoric acid 10mL mixing, need filter rear use such as muddiness;
Hydrochloric acid (5+95): 5mL hydrochloric acid is poured in the 95mL water into mixing;
Titanium trichloride solution (1+9): get titanium trichloride 15 at %～20 at % solution, put into amber bottle, with hydrochloric acid (5+95) dilution, add the protection of one deck whiteruss behind the mixing;
The potassium dichromate standard solution, c (1/6K
2Cr
2O
7)=0.1mol/L;
Diphenylamine sulfonic acid sodium salt indicator: 0.2 at %;
Sulfuric acid (5+95): 50mL sulfuric acid is poured in the 950mL water into mixing;
Iron ammonium sulfate standard solution (about 0.1mol/L): claim iron ammonium sulfate 19.7g, in the vitriolization (5+95), move in the 1000mL volumetric flask that (5+95) is diluted to scale, mixing with sulfuric acid.
Embodiment 1
With 1
#Broken, the grinding of Fe-Ce intermediate alloy sample, making it become granularity is 80 purpose samples.
Take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 20mL, / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, add the 20mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, the results are shown in Table 8.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Computing formula is:
The mass percent of W in the formula (Fe)-iron, %;
The concentration numerical value of C-potassium dichromate standard solution, mol/L;
V
0Consume the volume numerical value of potassium dichromate standard solution during-titration blank solution, mL;
Consume the volume numerical value of potassium dichromate standard solution during V-titration sample, mL;
The quality numerical value of m-sample, g;
55.85 the molal weight of-iron, g/mol.
Embodiment 2
With 2
#Broken, the grinding of Fe-Ce intermediate alloy sample, making it become granularity is 80 purpose samples.
Take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 25mL, / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, add the 20mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 5 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 8 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Embodiment 3
With 3
#Broken, the grinding of Fe-Ce intermediate alloy sample, making it become granularity is 80 purpose samples.
Take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 22mL, / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, add the 25mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 8 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Embodiment 4
Take by weighing sample 0.1000g1
#Fe-Ce intermediate alloy sample is in the triangular flask of 300mL, add the iron standard solution that is equivalent to 5.00 at % in the 0.1000g sample, add (2+3) mixture of sulfuric phosphoric acid 25mL, / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, add the 25mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 7 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Embodiment 5
Take by weighing sample 0.1000g3
#Fe-Ce intermediate alloy sample is in the triangular flask of 300mL, add the iron standard solution that is equivalent to 5.00 at % in the 0.1000g sample, take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 20mL, take off at 1/2nd bottle height places at the bottom of the high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, slightly cold, add the 25mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 8 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Embodiment 6
Take by weighing sample 0.1000g3
#Fe-Ce intermediate alloy sample is in the triangular flask of 300mL, add the iron standard solution that is equivalent to 10.00 at % in the 0.1000g sample, take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 20mL, take off at 1/2nd bottle height places at the bottom of the high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, slightly cold, add the 25mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 8 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Embodiment 7
Take by weighing the 0.0900g high purity iron in the triangular flask of 300mL, add the cerium standard solution that is equivalent to 10.00 at % in the 0.1000g sample, take by weighing sample 0.1000g in the triangular flask of 300mL, add (2+3) mixture of sulfuric phosphoric acid 22mL, take off at 1/2nd bottle height places at the bottom of the high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, slightly cold, add the 25mL of (1+1) hydrochloric acid, heat at electric furnace, with inferior solution of tin 6 at% of dichloride to light yellow (do not boil after the reduction and should bleach).Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 10 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band, computing formula the results are shown in Table 8 with embodiment 1.
Determining of blank value: only before titration, add 6.00mL iron ammonium sulfate standard solution (c 0.1mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number.
Table 8: measurement result at %
| Sample | Element | Asserting value | Measured value |
| Fe-Ce intermediate alloy 1 #Sample | Fe | ／ | 90.15 |
| Fe-Ce intermediate alloy 2 #Sample | Fe | ／ | 97.95 |
| Fe-Ce intermediate alloy 3 #Sample | Fe | ／ | 86.10 |
| Fe-Ce1 #Sample+5.00 at % iron | Fe | 95.15 | 95.25 |
| Fe-Ce3 #Sample+5.00 at % iron | Fe | 91.10 | 91.20 |
| Fe-Ce3 #Sample+10.00 at % iron | Fe | 96.10 | 95.85 |
| 0.0900g high purity iron+10.00 at % ceriums | Fe | 89.98 | 90.10 |
[0098]?
Claims (1)
1. the assay method of iron content in the Fe-Ce intermediate alloy is characterized in that sample is broken, be ground to its granularity is 80 orders, and determination step is as follows:
1), the mixture of sulfuric phosphoric acid of adding (2+3) mixture of sulfuric phosphoric acid 15mL～25mL(2+3 is that the sulfuric acid 40mL of ρ 1.84g/mL and the phosphoric acid 60mL of ρ 1.685g/mL are stirred evenly), / 2nd bottle height places at the bottom of high-temperature electric resistance furnace heating makes sample be dissolved to concentrated sulphuric acid cigarette fully to leave bottle, take off, slightly cold, the hydrochloric acid that adds the 20mL～30mL(1+1 of (1+1) hydrochloric acid is that the hydrochloric acid 50mL of ρ 1.19g/mL and the water of 50mL are stirred evenly), heat at electric furnace, with the inferior solution of tin of dichloride (6 at%) to light yellow (do not boil after the reduction and should bleach); Take off, slightly cold, heating water 50mL(solution remains on 40～50 ℃), add 8 sodium tungstates, drip titanium trichloride solution to stable blueness, be titrated to blue the disappearance with the potassium dichromate standard solution, add immediately 4～5 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution and stablize purple and do not move back and be terminal point, blank in company with band;
2), determining of blank value: in the blank solution of companion sample manipulation, add 6.00mL iron ammonium sulfate standard solution c (FeSO
4=0.1 mol/L), 4 diphenylamine sulfonic acid sodium salt indicator, be titrated to the potassium dichromate standard solution immediately and stablize purple and do not move back and be terminal point, write down a milliliter number A, in solution, add 6.00mL iron ammonium sulfate standard solution again, be titrated to take the potassium dichromate standard solution again and stablize purple and do not move back as terminal point and write down milliliter number B, then a V
0=A-B is blank milliliter number;
Computing formula is:
The mass percent of W in the formula (Fe)-iron, %;
The concentration numerical value of C-potassium dichromate standard solution, mol/L;
V
0Consume the volume numerical value of potassium dichromate standard solution during-titration blank solution, mL;
Consume the volume numerical value of potassium dichromate standard solution during V-titration sample, mL;
The quality numerical value of m-sample, g;
55.85 the molal weight of-iron, g/mol.
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| CN103969202A (en) * | 2014-05-12 | 2014-08-06 | 马钢(集团)控股有限公司 | Method for detecting content of total iron in iron ore through automatic potentiometric titration of photometric electrode |
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| CN107462665A (en) * | 2017-07-07 | 2017-12-12 | 泉州众志金刚石工具有限公司 | The assay method of iron content in a kind of iron copper and tin ternary pre-alloyed powder |
| CN109342644A (en) * | 2018-09-30 | 2019-02-15 | 承德建龙特殊钢有限公司 | The detection method of all iron content in a kind of vanadium titanium valve |
| CN109580872A (en) * | 2018-12-11 | 2019-04-05 | 天津冶金集团中兴盛达钢业有限公司 | Bivalent cupric ion rapid assay methods in a kind of copper plating bath |
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| CN109580872A (en) * | 2018-12-11 | 2019-04-05 | 天津冶金集团中兴盛达钢业有限公司 | Bivalent cupric ion rapid assay methods in a kind of copper plating bath |
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