CN107436290A - The assay method of chromium content in a kind of vananum - Google Patents
The assay method of chromium content in a kind of vananum Download PDFInfo
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- CN107436290A CN107436290A CN201710884645.XA CN201710884645A CN107436290A CN 107436290 A CN107436290 A CN 107436290A CN 201710884645 A CN201710884645 A CN 201710884645A CN 107436290 A CN107436290 A CN 107436290A
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- vananum
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- chromium content
- assay method
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- 239000011651 chromium Substances 0.000 title claims abstract description 80
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 74
- 238000003556 assay Methods 0.000 title claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 44
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000706 filtrate Substances 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 238000002835 absorbance Methods 0.000 claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 29
- 238000012360 testing method Methods 0.000 claims abstract description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- GDEBSAWXIHEMNF-UHFFFAOYSA-O cupferron Chemical compound [NH4+].O=NN([O-])C1=CC=CC=C1 GDEBSAWXIHEMNF-UHFFFAOYSA-O 0.000 claims abstract description 18
- 230000003647 oxidation Effects 0.000 claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 12
- 238000012545 processing Methods 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- 239000006166 lysate Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 42
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 16
- 229910052720 vanadium Inorganic materials 0.000 claims description 16
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 16
- 235000019504 cigarettes Nutrition 0.000 claims description 13
- 239000012085 test solution Substances 0.000 claims description 11
- 239000012086 standard solution Substances 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 235000010290 biphenyl Nutrition 0.000 claims description 8
- 239000004305 biphenyl Substances 0.000 claims description 8
- 125000006267 biphenyl group Chemical group 0.000 claims description 8
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 8
- 230000001186 cumulative effect Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- ZAOCWQZQPKGTRN-UHFFFAOYSA-N nitrous acid;sodium Chemical compound [Na].ON=O ZAOCWQZQPKGTRN-UHFFFAOYSA-N 0.000 claims 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 abstract description 10
- 238000001514 detection method Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000012286 potassium permanganate Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 235000010344 sodium nitrate Nutrition 0.000 description 3
- 239000004317 sodium nitrate Substances 0.000 description 3
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 description 2
- 244000061458 Solanum melongena Species 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 241000165940 Houjia Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- -1 heating is boiled Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- ZBJWWKFMHOAPNS-UHFFFAOYSA-N loretin Chemical compound C1=CN=C2C(O)=C(I)C=C(S(O)(=O)=O)C2=C1 ZBJWWKFMHOAPNS-UHFFFAOYSA-N 0.000 description 1
- 229950010248 loretin Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical class [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses a kind of assay method of chromium content in vananum, belong to technical field of analysis and detection.Methods described includes：Vananum sample is weighed, adding 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum lysate；Add ammonium persulfate solution heating to boil, cupferron is added after cooling, it is then dry to be filtrated to get containing Cr3+Filtrate；Nitrification processing is carried out after being carbonized to filtrate；Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, urea liquid is added after cooling, is added natrium nitrosum to solution colour and is disappeared, moves into constant volume in volumetric flask, obtain oxidation solution；Divide and take partial oxidation liquid in volumetric flask, add indicator, constant volume obtains prepare liquid, and tests absorbance；Draw standard working curve；Chromium content in vananum sample is obtained according to the absorbance and standard working curve measured.For this method without using ICP spectrometers, testing cost is low, and it is easy to operate, reproducible, accuracy is high.
Description
Technical field
The present invention relates to technical field of analysis and detection, the assay method of chromium content in more particularly to a kind of vananum.
Background technology
Vananum be it is a kind of produce the important element additive of titanium alloy, its host element chemical composition content and as miscellaneous
The content of prime element chromium generally requires to carry out in process of production strict control, chromium content number not only influence aluminium vanadium
Grade, the grade of alloy, it is often more important that easily have a strong impact on titanium alloy in titanium alloy grain boundaries segregation after being brought into as additive
Performance.So in vananum is produced, the control to chromium is particularly important, and in vananum a large amount of vanadium presence pair
The measure of chromium has interference, mainly carries out analysis detection by instrument ICP spectrometers at present, its accuracy of detection can reach 0.3% with
Under, and ICP spectrometers need to be purchased using the method detection, expense and consumptive material are more expensive, and in general medium-sized and small enterprises are difficult to.It is right
The detection of chromium content in vananum, under the premise of ensureing that measurement result is accurate, low content chromium especially in vananum
Detection, there is no preferable, economic chemical method to follow.
The content of the invention
It is an object of the invention to provide a kind of assay method of chromium content in vananum, this method is without using ICP light
Spectrometer and consumptive material, testing cost is low, and it is easy to operate, reproducible, accuracy is high.
To achieve the above object, the invention provides a kind of assay method of chromium content in vananum, including：
Vananum sample is weighed, adding 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum dissolving
Liquid；
Ammonium persulfate solution heating is added into the vananum lysate to boil, and cupferron is added after cooling, so
It is dry afterwards to be filtrated to get containing Cr3+Filtrate；
Nitrification processing is carried out after being carbonized to the filtrate；
Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea liquid is added after cooling, adds Asia
Sodium nitrate to solution colour disappears, and moves into constant volume in volumetric flask, obtains oxidation solution；
Divide and take the part oxidation solution in volumetric flask, add the hydrazine indicator of diphenyl phosphinylidyne two, constant volume, obtain prepare liquid,
Test absorbance of the prepare liquid at wavelength 540nm；
Prepare chromium standard solution and draw standard working curve；
The chromium content in vananum sample is obtained according to the absorbance measured and the standard working curve.
Further, the screen size of the vananum sample is less than 100 mesh.
Further, the quality of the vananum sample is 0.1000g~0.2000g.
Further, the vananum sample and 1+1 sulfuric acid, quality-volume ratio of 1+1 nitric acid are 1g:128~
144mL:72~96mL, preferably 1g:136mL:80mL.
Further, the concentration of the ammonium persulfate solution is 200g/L, and addition is that every gram of vananum sample adds
40~80mL.
Further, the concentration of the cupferron is 65g/L, and addition is that every gram of vananum sample adds 80mL.
Further, nitrification processing is carried out after the carbonization to the filtrate, is specially：To filtrate heating carbonization extremely
Sulfuric acid cigarette is emitted, removes cooling；Add the concentrated nitric acid 2~3min that is heated to smoldering to complete once to nitrify, nitrification number is more than 3 times.
Further, the time that the liquor potassic permanganate heating is boiled is 3~4min.
Further, the chromium content in the vananum sample calculates with specific reference to following formula：
In formula, WCrFor the chromium content in vananum sample；A is the absorbance of prepare liquid；A0For reagent blank absorbance；
K is the slope of standard working curve；V0For test solution cumulative volume, unit mL；V1For point test solution volume taken, unit mL；m0For
The quality of vananum sample, unit g.
Further, the assay method is applied to vananum examination of the chromium content between 0.01%~0.3%
Sample.
One or more of the embodiment of the present application technical scheme, has at least the following technical effects or advantages：
The assay method of chromium content in the vananum that the embodiment of the present application provides, including：Vananum sample is weighed, is added
Entering 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum lysate；Add into the vananum lysate
Enter ammonium persulfate solution heating to boil, cupferron is added after cooling, it is then dry to be filtrated to get containing Cr3+Filtrate；To the filter
Nitrification processing is carried out after liquid carbonization；Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea is added after cooling
Solution, add natrium nitrosum to solution colour and disappear, move into constant volume in volumetric flask, obtain oxidation solution；Divide and take the part oxygen
Change liquid in volumetric flask, add the hydrazine indicator of diphenyl phosphinylidyne two, constant volume, obtain prepare liquid, test the prepare liquid in wavelength
Absorbance at 540nm；Prepare chromium standard solution and draw standard working curve；According to the absorbance and the standard work measured
Make the chromium content in curve acquisition vananum sample.In this way, by the content of chromium in chemical gauging vananum, without
Using ICP spectrometers and consumptive material, testing cost is low, and it is easy to operate, reproducible, accuracy is high.
Brief description of the drawings
Fig. 1 is the assay method flow chart of chromium content in vananum provided in an embodiment of the present invention.
Embodiment
The embodiment of the present application provides a kind of assay method of chromium content in vananum, and this method is without using ICP spectrum
Instrument and consumptive material, testing cost is low, and it is easy to operate, reproducible, accuracy is high, not volatile, nontoxic, the green ring of detection reagent
Protect.
To achieve the above object, the embodiment of the present application general thought is as follows：
This application provides a kind of assay method of chromium content in vananum, including：
Vananum sample is weighed, adding 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum dissolving
Liquid；
Ammonium persulfate solution heating is added into the vananum lysate to boil, and cupferron is added after cooling, so
It is dry afterwards to be filtrated to get containing Cr3+Filtrate；
Nitrification processing is carried out after being carbonized to the filtrate；
Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea liquid is added after cooling, adds Asia
Sodium nitrate to solution colour disappears, and moves into constant volume in volumetric flask, obtains oxidation solution；
Divide and take the part oxidation solution in volumetric flask, add the hydrazine indicator of diphenyl phosphinylidyne two, constant volume, obtain prepare liquid,
Test absorbance of the prepare liquid at wavelength 540nm；
Prepare chromium standard solution and draw standard working curve；
The chromium content in vananum sample is obtained according to the absorbance measured and the standard working curve.
By the above as can be seen that the application makes vananum sample using the mixed acid of 1+1 sulfuric acid and 1+1 nitric acid
Dissolving, and Low Valent Vanadium is oxidized to pentavalent vanadium by ammonium persulfate, then the impurity elements such as vanadium are removed using cupferron to arrange
Remaining cupferron is removed except the interference to test result, then by nitrification processing, finally using potassium permanganate by Cr in solution3+
It is oxidized to Cr6+, the absorbance of solution is tested after removing unnecessary potassium permanganate, and compare chromium standard working curve and obtain vananum
In chromium content；This method ensure that the abundant dissolving of sample, and interference of the impurity element to test result is eliminated, without making
With ICP spectrometers and consumptive material, testing cost is low, and it is easy to operate, reproducible, accuracy is high.
In order to be better understood from above-mentioned technical proposal, below by accompanying drawing and specific embodiment to technical scheme
It is described in detail, it should be understood that the specific features in the embodiment of the present application and embodiment are to the detailed of technical scheme
Thin explanation, rather than the restriction to technical scheme, in the case where not conflicting, the embodiment of the present application and embodiment
In technical characteristic can be combined with each other.
The embodiment of the present application provides a kind of assay method of chromium content in vananum, and the measure that is particularly suitable for use in chromium contains
The vananum sample between 0.01%~0.3% is measured, as shown in figure 1, comprising the following steps：
Step S110：Vananum sample is weighed, adding 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vanadium aluminium
Alloy lysate；
Preferably, the screen size of the vananum sample is less than 100 mesh.The screen size refers to that sample can lead to
Cross the screen size of screen cloth.Suitable granularity is advantageous to the dissolving of sample, the excessive dissolving for being unfavorable for sample of granularity, eventually shadow
Ring the accuracy of test.
Preferably, the quality of the vananum sample is 0.1000g~0.2000g.Sample mass is favourable in this scope
In test operation, quality is excessive, then acid solution volume increase needed for dissolving, is unfavorable for subsequent operation.
In the present embodiment, the vananum sample is 1g with 1+1 sulfuric acid, quality-volume ratio of 1+1 nitric acid:128~
144mL:72~96mL, preferably 1g:136mL:80mL.Vananum uses 1+1 sulfuric acid and 1+1 nitric acid mixed acid compared with indissoluble solution
Sample can be dissolved, and the ratio can be such that vananum sample fully dissolves, and ensure that test result is accurate, overcome vanadium aluminium
Alloy it is more difficult fully dissolving the problem of.
Step S120：Ammonium persulfate solution is added into the vananum lysate, heating is boiled, and copper is added after cooling
Ferron, it is then dry to be filtrated to get containing Cr3+Filtrate；
Specifically, it is to make Low Valent Vanadium (divalence, trivalent, tetravalence) fully oxidized to add the purpose that ammonium persulfate heating is boiled
, then under strongly acidic conditions can be by pentavalent vanadium, ferric iron precipitation without precipitating trivalent chromium using cupferron into pentavalent vanadium
Property, vanadium is gone divided by interference of the despumation element to chrome determination.
Preferably, the concentration of the ammonium persulfate solution is 200g/L, and addition is that every gram of vananum sample adds 40
~80mL.The concentration of the cupferron is 65g/L, and addition is that every gram of vananum sample adds 80mL, and this dosage can protect
Card is cleared by vanadium, and otherwise remaining vanadium can influence last colour developing, make test result relatively low.
Step S130：Nitrification processing is carried out after being carbonized to the filtrate；
In the present embodiment, in order to exclude remaining cupferron to the interference of test, it is necessary to filtrate carry out nitrification processing with
Remove remaining cupferron.And it is the Ran Houjia in order to which remnants cupferron is changed into carbide that carbonization is first carried out before nitrification
Enter nitric acid and carry out nitrification processing removal carbide, so that subsequently nitrification is more complete, eliminate the remnants because of cupferron to test
As a result influence.Specifically, first to filtrate heating carbonization to sulfuric acid cigarette is emitted, cooling is removed；Then concentrated nitric acid is added to add
Heat is completed once to nitrify to the 2~3min that smolders, and concentrated nitric acid is added after cooling and is heated to 2~3min, second of nitre of completion of smoldering
Change, nitrification number is more than 3 times, and the filtrate after nitrification is white, to ensure that cupferron removes completely.If nitrification is endless
It is full-time, with the presence of remaining cupferron solution may be made to turn to be yellow, cause measurement result inaccurate.Wherein, heating uses electric furnace
Heating.
Step S140：Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea liquid is added after cooling,
Add natrium nitrosum to solution colour to disappear, then move into constant volume in volumetric flask, obtain oxidation solution；
In the present embodiment, in order to by Cr3+It is oxidized to Cr6+, add liquor potassic permanganate heating and boil, the time boiled is 3
~4min, keep untill the red of potassium permanganate do not move back, making chromium oxidation complete.It is to decompose excessive Asia to add urea liquid
Sodium nitrate, and add urea to be because natrium nitrosum has reproducibility before natrium nitrosum is added, prevent excessive natrium nitrosum will
Oxidized chromium is reduced at a low price again.The purpose for adding natrium nitrosum is to neutralize potassium permanganate.
Step S150：Divide and take the part oxidation solution in volumetric flask, the hydrazine indicator of addition diphenyl phosphinylidyne two, constant volume,
Prepare liquid is obtained, tests absorbance of the prepare liquid at wavelength 540nm；
Step S160：Prepare chromium standard solution and draw standard working curve；
Step S170：The chromium in vananum sample is obtained according to the absorbance measured and the standard working curve to contain
Amount.
In the present embodiment, the chromium content in the vananum sample calculates with specific reference to following formula：
In formula, WCrFor the chromium content in vananum sample；A is the absorbance of prepare liquid；A0For reagent blank absorbance；
K is the slope of standard working curve；V0For test solution cumulative volume, unit mL；V1For point test solution volume taken, unit mL；m0For
The quality of vananum sample, unit g.
It should be noted that step S160 can be carried out before or after any one step in step S110-S150,
For example, can be carried out before step S110, can also carry out after step s 140.
It is for a more detailed description to the application by the following examples.These embodiments are only to the optimal embodiment party of the present invention
The description of formula, there is not any limitation to the scope of the present invention.
Embodiment 1
S210：Weigh 0.1250g (m0) vananum sample 1 (AlV55) that chromium content is 0.040%, add nitric acid (1+
1) 10mL, sulfuric acid (1+1) 17mL, cap upper surface ware, are heated to emitting sulfuric acid 2~3min of cigarette, remove cooling, and 50mL is added along cup wall
Water, dissolve by heating salt；Heating can promote the dissolving of vananum.
S220：Add 10mL ammonium persulfates (200g/L) heating to boil to air pocket about 1~2min is emitted, make Low Valent Vanadium (two
Valency, trivalent, tetravalence) it is fully oxidized into pentavalent, cooling is removed, moves into 100mL volumetric flasks, scale is diluted to water, shaken up, body
Product is V10.Again 50mL (V are pipetted with pipette11) in 100mL volumetric flasks, add 10mL cupferrons (65g/L) side edged to shake anti-
Only localized precipitation produces, then is diluted with water to scale, shakes up, volume V20, stand 4~5min.Done with middling speed quantitative filter paper
Filter, obtains containing Cr3+Filtrate；
S230：Pipette filtrate 50mL (V21) be put into zeolite, cap upper surface ware in first heating carbonization on electric furnace to emitting sulfuric acid cigarette,
Remove cooling.Add 3mL concentrated nitric acids to be heated to emitting 2~3min of concentrated nitric acid cigarette completions nitrification for the first time, remove cooling；Add 3mL
Concentrated nitric acid is heated to emitting 2~3min of concentrated nitric acid cigarette completions, second of nitrification, removes cooling；3mL concentrated nitric acids are added to be heated to emitting
2~3min of concentrated nitric acid cigarette and the white completion third time nitrification of test solution, remove cooling.Wherein, the density of concentrated nitric acid be ρ=
1.42g/mL。
S240：The sample nitrified is added into water about 30mL in being heated on electric furnace along cup wall, increase potassium manganate solution boil 3~
4min, keep untill the red of potassium permanganate do not move back, making chromium oxidation complete, removing cooling.Add 5~10mL urea liquids (200g/
L the red for), then with natrium nitrosum (2g/L) being neutralized to potassium permanganate is decorporated in excessive 1 drop just, then moves into 100mL volumetric flasks
In, scale is diluted to water, shaken up, volume V30；With the dry filtering of middling speed quantitative filter paper；
S250：Divide and take 50mL (V31) filtrate in 100mL volumetric flasks, adds the hydrazine indicator of 3~4mL diphenyl phosphinylidyne two
(2.5g/L), aubergine complex is generated in solution, scale is diluted to water, shaken up, 10~20min is stood, in spectrophotometric
Count and absorbance A is surveyed at 540nm.
In order to exclude the mistake that the factors such as the pollution in the impurity in reagent, environment and operating process are come to sample measuring band
Difference, it is ensured that the accuracy of detection.Reagent blank experiment is analyzed simultaneously with sample, and assay method is identical with above-mentioned steps, measures suction
Luminosity is A0。
S260：Prepare chromium standard solution and draw standard working curve, specifically include following steps：
S261：Prepare chromium typical shelf solution：Weighing 0.2829g, in 105 DEG C of potassium bichromates for drying 2h, (benchmark tries in advance
Agent), dissolved with water, move into 1000mL volumetric flasks, be diluted with water to scale, mixed.This solution 1mL contains 100 μ g；
S262：Prepare chromium standard solution：Pipette 10.00mL chromium typical shelf solution and add 1mL sulfuric acid (1 in 100mL beakers
+ 1), then add 0.2g sodium sulfites, chromium is reduced to trivalent, then moved into 100mL volumetric flasks, being diluted to scale with water mixes,
This solution 1mL contains 10 μ g chromium；
S263：Draw standard working curve：Vananum test solution 1 (AlV55) is pipetted, six parts of 40mL, is respectively placed in one group
In 125mL conical flasks, 0mL, 0.20mL, 0.40mL, 0.60mL, 0.80mL chromium standard solution are separately added into, following steps are the same as examination
Sample operates, and using reagent blank as reference, its absorbance is surveyed at spectrophotometer wavelength 540nm, the results are shown in Table 1.With absorbance
For abscissa, chromium content is that ordinate draws standard working curve, obtains linear equation：Y=44.20x, R2=0.999.
The DIFFERENT Cr content standard solution absorbance test result of table 1
| Cr contents/μ g | 0 | 2 | 4 | 6 | 8 |
| Absorbance | 0 | 0.044 | 0.087 | 0.137 | 0.182 |
S270：According to the absorbance measured and obtained standard working curve, the chromium calculated in vananum sample contains
Amount：
Wherein,V11、V21、V31Respectively divide the test solution volume taken every time, be divided into and taken 3
It is secondary；V10、V20、V30For the cumulative volume divided every time after taking test solution constant volume.
Test 8 times and average, test result is shown in Table 2.
Embodiment 2
S310：Weigh 0.1250g (m0) vananum sample 2 (AlV55) that chromium content is 0.100%, add nitric acid (1+
1) 10mL, sulfuric acid (1+1) 17mL, cap upper surface ware, are heated to emitting sulfuric acid 2~3min of cigarette, remove cooling, and 50mL is added along cup wall
Water, dissolve by heating salt；
S320：Add 10mL ammonium persulfates (200g/L) heating to boil to air pocket about 1~2min is emitted, make Low Valent Vanadium (two
Valency, trivalent, tetravalence) it is fully oxidized into pentavalent, cooling is removed, moves into 100mL volumetric flasks, scale is diluted to water, shaken up, body
Product is V10.Again 50mL (V are pipetted with pipette11) in 100mL volumetric flasks, add 10mL cupferrons (65g/L) side edged to shake anti-
Only localized precipitation produces, then is diluted with water to scale, shakes up, volume V20, stand 4~5min.Done with middling speed quantitative filter paper
Filter, obtains containing Cr3+Filtrate；
S330：Pipette filtrate 50mL (V21) be put into zeolite, cap upper surface ware in first heating carbonization on electric furnace to emitting sulfuric acid cigarette,
Remove cooling.Add 3mL concentrated nitric acids to be heated to emitting 2~3min of concentrated nitric acid cigarette completions nitrification for the first time, remove cooling；Add 3mL
Concentrated nitric acid is heated to emitting 2~3min of concentrated nitric acid cigarette completions, second of nitrification, removes cooling；3mL concentrated nitric acids are added to be heated to emitting
2~3min of concentrated nitric acid cigarette and the white completion third time nitrification of test solution, remove cooling.Wherein, the density of concentrated nitric acid be ρ=
1.42g/mL。
S340：The sample nitrified is added into water about 30mL in being heated on electric furnace along cup wall, increase potassium manganate solution boil 3~
4min, keep untill the red of potassium permanganate do not move back, making chromium oxidation complete, removing cooling.Add 5mL urea liquids (200g/L),
The red that potassium permanganate is neutralized to natrium nitrosum (2g/L) again is decorporated in excessive 1 drop just, then is moved into 100mL volumetric flasks,
Scale is diluted to water, shaken up, volume V30.With the dry filtering of middling speed quantitative filter paper, initial filtrate is abandoned or adopted.
S350：Divide and take 50mL (V31) filtrate in 100mL volumetric flasks, adds the hydrazine indicator (2.5g/ of 3mL diphenyl phosphinylidyne two
L), aubergine complex is generated in solution, scale is diluted to water, shaken up, 10~20min is stood, in spectrophotometer 540nm
Place surveys absorbance A.
In order to exclude the mistake that the factors such as the pollution in the impurity in reagent, environment and operating process are come to sample measuring band
Difference, it is ensured that the accuracy of detection.Reagent blank experiment is analyzed simultaneously with sample, and assay method is identical with above-mentioned steps, measures suction
Luminosity is A0。
S360：The standard working curve that absorbance and embodiment 1 according to measuring obtains, calculate in vananum sample
Chromium content, circular is same as Example 1.Test 8 times and average, the results are shown in Table 2.
Chromium content test result in the vananum sample of table 2
By embodiment 1,2 respectively to chromium content be 0.040%, 0.100% vananum sample (AlV55) chromium content
It is measured, the results showed that the assay method degree of accuracy of the application, precision are higher, and relative standard deviation is all very low.
One or more of embodiment of the present invention technical scheme, has at least the following technical effects or advantages：
The assay method of chromium content in the vananum that the embodiment of the present application provides, including：Vananum sample is weighed, is added
Entering 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum lysate；Add into the vananum lysate
Enter ammonium persulfate solution heating to boil, cupferron is added after cooling, it is then dry to be filtrated to get containing Cr3+Filtrate；To the filter
Nitrification processing is carried out after liquid carbonization；Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea is added after cooling
Solution, add natrium nitrosum to solution colour and disappear, move into constant volume in volumetric flask, obtain oxidation solution；Divide and take the part oxygen
Change liquid in volumetric flask, add the hydrazine indicator of diphenyl phosphinylidyne two, constant volume, obtain prepare liquid, test the prepare liquid in wavelength
Absorbance at 540nm；Prepare chromium standard solution and draw standard working curve；According to the absorbance and the standard work measured
Make the chromium content in curve acquisition vananum sample.In this way, by the content of chromium in chemical gauging vananum, without
Using ICP spectrometers and consumptive material, testing cost is low, and it is easy to operate, reproducible, accuracy is high.
It should be noted last that above embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (10)
- A kind of 1. assay method of chromium content in vananum, it is characterised in that including：Vananum sample is weighed, adding 1+1 sulfuric acid and 1+1 nitric acid makes sample fully decompose, and obtains vananum lysate；Ammonium persulfate solution heating is added into the vananum lysate to boil, and cupferron, Ran Hougan are added after cooling It is filtrated to get and contains Cr3+Filtrate；Nitrification processing is carried out after being carbonized to the filtrate；Liquor potassic permanganate heating is added into the filtrate after nitrification to boil, and urea liquid is added after cooling, adds nitrous acid Sodium to solution colour disappears, and moves into constant volume in volumetric flask, obtains oxidation solution；Divide and take the part oxidation solution in volumetric flask, add the hydrazine indicator of diphenyl phosphinylidyne two, constant volume, obtain prepare liquid, test Absorbance of the prepare liquid at wavelength 540nm；Prepare chromium standard solution and draw standard working curve；The chromium content in vananum sample is obtained according to the absorbance measured and the standard working curve.
- 2. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the vananum sample Screen size be less than 100 mesh.
- 3. the assay method of chromium content in vananum as claimed in claim 2, it is characterised in that the vananum sample Quality be 0.1000g~0.2000g.
- 4. the assay method of chromium content in the vananum as described in one of claim 1-3, it is characterised in that the vanadium aluminium closes Golden sample is 1g with 1+1 sulfuric acid, quality-volume ratio of 1+1 nitric acid:128~144mL:72~96mL, preferably 1g:136mL: 80mL。
- 5. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the ammonium persulfate solution Concentration be 200g/L, addition is that every gram of vananum sample adds 40~80mL.
- 6. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the cupferron it is dense It is that every gram of vananum sample adds 80mL to spend for 65g/L, addition.
- 7. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that described to the filtrate carbon Nitrification processing is carried out after change, is specially：To filtrate heating carbonization to sulfuric acid cigarette is emitted, cooling is removed；Add concentrated nitric acid heating Complete once to nitrify to the 2~3min that smolders, nitrification number is more than 3 times.
- 8. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the liquor potassic permanganate It is 3~4min to heat the time boiled.
- 9. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the vananum sample In chromium content with specific reference to following formula calculate：<mrow> <msub> <mi>W</mi> <mrow> <mi>C</mi> <mi>r</mi> </mrow> </msub> <mo>=</mo> <mfrac> <mrow> <mo>(</mo> <mi>A</mi> <mo>-</mo> <msub> <mi>A</mi> <mn>0</mn> </msub> <mo>)</mo> <mo>&times;</mo> <mi>K</mi> <mo>&times;</mo> <msub> <mi>V</mi> <mn>0</mn> </msub> <mo>&times;</mo> <msup> <mn>10</mn> <mrow> <mo>-</mo> <mn>6</mn> </mrow> </msup> </mrow> <mrow> <msub> <mi>m</mi> <mn>0</mn> </msub> <mo>&times;</mo> <msub> <mi>V</mi> <mn>1</mn> </msub> </mrow> </mfrac> <mo>&times;</mo> <mn>100</mn> <mi>%</mi> </mrow>In formula, WCrFor the chromium content in vananum sample；A is the absorbance of prepare liquid；A0For reagent blank absorbance；K is The slope of standard working curve；V0For test solution cumulative volume, unit mL；V1For point test solution volume taken, unit mL；m0For vanadium The quality of aluminum alloy specimen, unit g.
- 10. the assay method of chromium content in vananum as claimed in claim 1, it is characterised in that the assay method is fitted For vananum sample of the chromium content between 0.01%~0.3%.
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| CN111537497A (en) * | 2020-04-26 | 2020-08-14 | 山东莱钢永锋钢铁有限公司 | Method for measuring content of chromium sesquioxide in drainage sand |
| CN113418907A (en) * | 2021-07-26 | 2021-09-21 | 中车大连机车车辆有限公司 | Method for dissolving cast iron material and method for detecting element content in cast iron |
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