CN103645189A - Method for simultaneously measuring Cr, Ni and Ti in stainless steel 1Cr18Ni9Ti - Google Patents
Method for simultaneously measuring Cr, Ni and Ti in stainless steel 1Cr18Ni9Ti Download PDFInfo
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- CN103645189A CN103645189A CN201310644007.2A CN201310644007A CN103645189A CN 103645189 A CN103645189 A CN 103645189A CN 201310644007 A CN201310644007 A CN 201310644007A CN 103645189 A CN103645189 A CN 103645189A
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Abstract
The invention belongs to the technical field of aeronautical materials, and particularly relates to a method for simultaneously measuring Cr, Ni and Ti in stainless steel 1Cr18Ni9Ti. The method comprises the steps of measuring the Cr by a hydrochloric acid method, measuring Ni by a high-Cr steel Ni reagent colorimetric method, and measuring Ti by an antipyrine methane colorimetric method. According to the method, the measurement of the Cr, the Ni and the Ti in the stainless steel can be integrated, the samples are weighed and dissolved in a unified way, and then the samples are respectively tested after being separated, so that the original complicated steps are reduced, the time and the cost are saved, and the testing efficiency is greatly increased.
Description
Technical field
The invention belongs to aeronautical material technical field, particularly relate to a kind of method of chromium, nickel, titanium simultaneous determination in stainless steel 1Cr18Ni9Ti.
Background technology
In the test chemical method of existing stainless steel 1Cr18Ni9Ti composition, chromium, nickel, titanium have respectively method of testing, and common analysis has:
1, ammonium persulfate oxidation volumetric method is measured chromium amount.Sample, with after sulfuric acid dissolution, drips nitric acid oxidation.In sulfuric acid, phosphoric acid medium, take silver nitrate as catalyzer, with ammonium persulfate, chromium is oxidized to sexavalence, with the titration of iron ammonium sulfate volumetric soiutions.
2, fourth dioxime colorimetric method for determining nickel amount.Sample, with after sulfuric acid dissolution, drips nitric acid oxidation.Add sodium potassium tartrate tetrahydrate and sodium hydroxide solution, remove the interference of the metallic ion that is insoluble to alkaline solution.Under alkaline environment, oxygenant ammonium persulfate is oxidized to tetravalence by nickel, generates red complex ion, whereby colorimetric with the effect of fourth dioxime.
3, diantipyry methane spectrophotometry is measured titanium amount.Sample dissolves with the sal prunella nitration mixture of suitable proportion, adds sulfuric acid and is evaporated to and emits sulfuric acid cigarette.After dissolving, in 1.2～3.6moL/L hydrochloric acid medium, iron reduces with ascorbic acid, and titanium and diantipyrylmethane generate yellow complex, measure its absorbance.
Consulting in related data and have stainless continuous rapid analysis, is generally with the molten sample of chloroazotic acid.But in the mensuration of element, chromium adopts chromic acid colourimetry, and wherein the consumption of EDTA will strictly be controlled, and in the time of not, result is higher, Lower result when excessive, bad grasp, not as ammonium persulfate oxidation volumetric method is stablized; Nickel adopts fourth dioxime colourimetry; Titanium adopts hydrogen peroxide colourimetry.
Method for measuring weak point is respectively need to take respectively sample dissolve and measure, and step is more loaded down with trivial details, and the test period is long, and experimentation cost is high.The weak point of existing continuous rapid analysis is that the method stability of using is not so good as the stability of method for measuring respectively.
Summary of the invention
Goal of the invention: the invention provides a kind of method of chromium, nickel, titanium simultaneous determination in stainless steel 1Cr18Ni9Ti, can reduce original complicated step, save time and cost, greatly improved test efficiency.
Technical scheme: a kind of method of chromium, nickel, titanium simultaneous determination in stainless steel 1Cr18Ni9Ti, comprises the following steps:
Step 1: take stainless steel 1Cr18Ni9Ti sample 0.25g in 250ml triangular flask, add 40ml sulfuric acid 1+4, dissolution in low temperature, drips ρ 1.42 nitric acid oxidations, boils and drives most nitrogen oxides, in cooling immigration 250ml volumetric flask, is diluted to scale with water;
Step 2: get solution 50.00ml that step 1 obtains in 500ml triangular flask, add mixture of sulfuric phosphoric acid 10.00ml, dissolution in low temperature adds 1.7% silver nitrate 5.00ml, 15% ammonium persulfate 15.00ml～20.00ml, boil to emitting air pocket, add 1+1 hydrochloric acid 1.00ml～2.00mL, boil 5～10min, condense to silver nitride precipitation, with flowing water, be cooled to room temperature immediately, 1+1 adds sulfuric acid 20.00mL, 3～5 of vanadium reagentses, use immediately the titration of 0.1mol/L iron ammonium sulfate, it is terminal that solution is transformed into bright green by cherry-red; Analysis result is calculated:
When band standard specimen calculates, by (1) formula, calculate the percentage composition of chromium:
Cr%=cV
1/V
2 （1）
In formula:
C--the percentage composition of standard specimen chromium;
V
1--sample consumes the volume of iron ammonium sulfate standard solution, ml;
V
2--standard specimen consumes the volume of iron ammonium sulfate standard solution, ml;
While converting with standard solution, by (2) formula, calculate the percentage composition of chromium;
Cr%=1.733cV/m (2)
In formula:
The amount of substance concentration of c--iron ammonium sulfate standard solution, mol/L;
V--during titration end-point, consume the volume of iron ammonium sulfate standard solution, ml;
M--sample weight, g;
Step 3, get in step 1 sample solution 10ml in 100ml volumetric flask, add 50% ammonium citrate solution 10.00ml, 0.05mol/L iodine liquid 6.00ml shakes up and places 2～5min, coloring solution: add 0.1% fourth dioxime 20.00ml, so that water is rare, shake up to scale, place 2～5min, with green color filter, 530nm wavelength, 0.5cm cuvette colorimetric; Analysis result is calculated, by (3) formula band standard specimen, calculates:
Ni%=cA1/A0 （3）
In formula:
C--the percentage composition of standard specimen nickel;
The absorbance of A1--style;
The absorbance of A0--standard specimen;
Step 4, minute get in step 1 sample solution 20.00ml in 100ml capacity, add 1+1 hydrochloric acid 15.00ml, add 5% ascorbic acid 10.00ml and shake up rear placement 5min, coloring solution: add 5% diantipyrylmethane 20./00ml, with water, be diluted to scale, after placing 30min, with 0.5cm～1cm cuvette, the wavelength of 430nm carries out colorimetric; Calculating to analysis result: calculate by (4) formula band standard specimen:
Ti%=cA
1/A
0 （4）
In formula:
C--the percentage composition of standard specimen titanium;
A
1--the absorbance of sample;
A
0--the absorbance of standard specimen.
Mixture of sulfuric phosphoric acid in step 2 is sulfuric acid+phosphoric acid+water: 150+170+700, and vanadium reagents is that benzene is for ortho-aminobenzoic acid indicator.
Beneficial effect
The present invention is integrated together the mensuration of chromium, nickel, titanium in stainless steel, unified sampling, and unified molten sample, through too getting test respectively, has reduced original complicated step again, has saved time and cost, has greatly improved test efficiency.
Embodiment
Below the present invention is described in further detail.
Basic ideas of the present invention are: sample, after dilute sulfuric acid dissolution in low temperature, drips nitric acid oxidation, moves into volumetric flask.Then divide and get 50ml in sulfuric acid, phosphoric acid medium, take silver nitrate as catalyzer, with ammonium persulfate, chromium is oxidized to sexavalence, with iron ammonium sulfate volumetric soiutions titration determination chromium element; Divide and get the elements such as 10ml test solution, adding citric acid ammonium Complexing Iron, cobalt, in alkaline medium, when having under oxygenant existence, nickel and fourth dioxime generate claret network and thing, whereby colorimetric estimation nickel element; Minute get 20ml test solution and eliminate ferric interference with ascorbic acid, in 10%～20% hydrochloric acid medium, diantipyrylmethane and titanium ion effect generation yellow complex, whereby colorimetric estimation titanium elements.
Basic operational steps of the present invention is:
The first step: with sulfuric acid (1+4) dissolution in low temperature sample, drip nitric acid oxidation, move into volumetric flask.
Second step: divide and get 50ml, survey chromium with ammonium persulfate oxidation volumetric method.
The 3rd step: divide and get 10ml, with dimethylglyoxime Spectrophotometry for Determination nickel.
The 4th step: divide and get 20ml, survey titanium with diantipyry methane spectrophotometry.
Concrete steps of the present invention are: a kind of method of chromium, nickel, titanium simultaneous determination in stainless steel 1Cr18Ni9Ti, comprises the following steps:
Step 1: take stainless steel 1Cr18Ni9Ti sample 0.25g in 250ml triangular flask, add 40ml sulfuric acid 1+4, dissolution in low temperature, drips ρ 1.42 nitric acid oxidations, boils and drives most nitrogen oxides, in cooling immigration 250ml volumetric flask, is diluted to scale with water;
Step 2: get solution 50.00ml that step 1 obtains in 500ml triangular flask, add mixture of sulfuric phosphoric acid 10.00ml, dissolution in low temperature adds 1.7% silver nitrate 5.00ml, 15% ammonium persulfate 15.00ml～20.00ml, boil to emitting air pocket, add 1+1 hydrochloric acid 1.00ml～2.00mL, boil 5～10min, condense to silver nitride precipitation, with flowing water, be cooled to room temperature immediately, 1+1 adds sulfuric acid 20.00mL, 3～5 of vanadium reagentses, use immediately the titration of 0.1mol/L iron ammonium sulfate, it is terminal that solution is transformed into bright green by cherry-red; Analysis result is calculated:
When band standard specimen calculates, by (1) formula, calculate the percentage composition of chromium:
Cr%=cV
1/V
2 （1）
In formula:
C--the percentage composition of standard specimen chromium;
V
1--sample consumes the volume of iron ammonium sulfate standard solution, ml;
V
2--standard specimen consumes the volume of iron ammonium sulfate standard solution, ml;
While converting with standard solution, by (2) formula, calculate the percentage composition of chromium;
Cr%=1.733cV/m (2)
In formula:
The amount of substance concentration of c--iron ammonium sulfate standard solution, mol/L;
V--during titration end-point, consume the volume of iron ammonium sulfate standard solution, ml;
M--sample weight, g;
Step 3, get in step 1 sample solution 10ml in 100ml volumetric flask, add 50% ammonium citrate solution 10.00ml, 0.05mol/L iodine liquid 6.00ml shakes up and places 2～5min, coloring solution: add 0.1% fourth dioxime 20.00ml, so that water is rare, shake up to scale, place 2～5min, with green color filter, 530nm wavelength, 0.5cm cuvette colorimetric; Analysis result is calculated, by (3) formula band standard specimen, calculates:
Ni%=cA1/A0 （3）
In formula:
C--the percentage composition of standard specimen nickel;
The absorbance of A1--style;
The absorbance of A0--standard specimen;
Step 4, minute get in step 1 sample solution 20.00ml in 100ml capacity, add 1+1 hydrochloric acid 15.00ml, add 5% ascorbic acid 10.00ml and shake up rear placement 5min, coloring solution: add 5% diantipyrylmethane 20./00ml, with water, be diluted to scale, after placing 30min, with 0.5cm～1cm cuvette, the wavelength of 430nm carries out colorimetric; Calculating to analysis result: calculate by (4) formula band standard specimen:
Ti%=cA
1/A
0 （4）
In formula:
C--the percentage composition of standard specimen titanium;
A
1--the absorbance of sample;
A
0--the absorbance of standard specimen.
Mixture of sulfuric phosphoric acid in step 2 is sulfuric acid+phosphoric acid+water: 150+170+700, and vanadium reagents is that benzene is for ortho-aminobenzoic acid indicator.
The present invention is integrated together the mensuration of chromium, nickel, titanium in stainless steel, unified sampling, and unified molten sample, through too getting test respectively, has reduced original complicated step again, has saved time and cost, has greatly improved test efficiency.
Claims (2)
1. a method for chromium, nickel, titanium simultaneous determination in stainless steel 1Cr18Ni9Ti, is characterized in that, comprises the following steps:
Step 1: take stainless steel 1Cr18Ni9Ti sample 0.25g in 250ml triangular flask, add 40ml sulfuric acid 1+4, dissolution in low temperature, drips ρ 1.42 nitric acid oxidations, boils and drives most nitrogen oxides, in cooling immigration 250ml volumetric flask, is diluted to scale with water;
Step 2: get solution 50.00ml that step 1 obtains in 500ml triangular flask, add mixture of sulfuric phosphoric acid 10.00ml, dissolution in low temperature adds 1.7% silver nitrate 5.00ml, 15% ammonium persulfate 15.00ml～20.00ml, boil to emitting air pocket, add 1+1 hydrochloric acid 1.00ml～2.00mL, boil 5～10min, condense to silver nitride precipitation, with flowing water, be cooled to room temperature immediately, 1+1 adds sulfuric acid 20.00mL, 3～5 of vanadium reagentses, use immediately the titration of 0.1mol/L iron ammonium sulfate, it is terminal that solution is transformed into bright green by cherry-red; Analysis result is calculated:
When band standard specimen calculates, by (1) formula, calculate the percentage composition of chromium:
Cr%=cV
1/V
2 （1）
In formula:
C--the percentage composition of standard specimen chromium;
V
1--sample consumes the volume of iron ammonium sulfate standard solution, ml;
V
2--standard specimen consumes the volume of iron ammonium sulfate standard solution, ml;
While converting with standard solution, by (2) formula, calculate the percentage composition of chromium;
Cr%=1.733cV/m (2)
In formula:
The amount of substance concentration of c--iron ammonium sulfate standard solution, mol/L;
V--during titration end-point, consume the volume of iron ammonium sulfate standard solution, ml;
M--sample weight, g;
Step 3, get in step 1 sample solution 10ml in 100ml volumetric flask, add 50% ammonium citrate solution 10.00ml, 0.05mol/L iodine liquid 6.00ml shakes up and places 2～5min, coloring solution: add 0.1% fourth dioxime 20.00ml, so that water is rare, shake up to scale, place 2～5min, with green color filter, 530nm wavelength, 0.5cm cuvette colorimetric; Analysis result is calculated, by (3) formula band standard specimen, calculates:
Ni%=cA1/A0 （3）
In formula:
C--the percentage composition of standard specimen nickel;
The absorbance of A1--style;
The absorbance of A0--standard specimen;
Step 4, minute get in step 1 sample solution 20.00ml in 100ml capacity, add 1+1 hydrochloric acid 15.00ml, add 5% ascorbic acid 10.00ml and shake up rear placement 5min, coloring solution: add 5% diantipyrylmethane 20./00ml, with water, be diluted to scale, after placing 30min, with 0.5cm～1cm cuvette, the wavelength of 430nm carries out colorimetric; Calculating to analysis result: calculate by (4) formula band standard specimen:
Ti%=cA
1/A
0 （4）
In formula:
C--the percentage composition of standard specimen titanium;
A
1--the absorbance of sample;
A
0--the absorbance of standard specimen.
2. the method for chromium, nickel, titanium simultaneous determination in a kind of stainless steel 1Cr18Ni9Ti according to claim 1, is characterized in that, the mixture of sulfuric phosphoric acid in step 2 is sulfuric acid+phosphoric acid+water: 150+170+700, and vanadium reagents is that benzene is for ortho-aminobenzoic acid indicator.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034722A (en) * | 2014-06-03 | 2014-09-10 | 江苏永钢集团有限公司 | Method for measuring substance content of composite silicon carbide |
| CN105588743A (en) * | 2015-12-17 | 2016-05-18 | 吴志强 | Sample dissolving method for testing titanium in pig iron and cast iron through diantipyrylmethane colorimetric method |
| CN105628691A (en) * | 2015-12-18 | 2016-06-01 | 抚顺罕王直接还原铁有限公司 | Method for measuring titanium content of iron ore |
| CN109358057A (en) * | 2018-12-27 | 2019-02-19 | 湖南中创化工股份有限公司 | A method of Ti content in measurement sec-butyl acetate device or sec-butyl alcohol device production sample |
| CN112557324A (en) * | 2020-12-07 | 2021-03-26 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring titanium mass content in steel |
| CN113237870A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting components of NiCr alloy |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034722A (en) * | 2014-06-03 | 2014-09-10 | 江苏永钢集团有限公司 | Method for measuring substance content of composite silicon carbide |
| CN105588743A (en) * | 2015-12-17 | 2016-05-18 | 吴志强 | Sample dissolving method for testing titanium in pig iron and cast iron through diantipyrylmethane colorimetric method |
| CN105628691A (en) * | 2015-12-18 | 2016-06-01 | 抚顺罕王直接还原铁有限公司 | Method for measuring titanium content of iron ore |
| CN109358057A (en) * | 2018-12-27 | 2019-02-19 | 湖南中创化工股份有限公司 | A method of Ti content in measurement sec-butyl acetate device or sec-butyl alcohol device production sample |
| CN112557324A (en) * | 2020-12-07 | 2021-03-26 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring titanium mass content in steel |
| CN113237870A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting components of NiCr alloy |
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Application publication date: 20140319 |