CN115950843A - Improved iodine oxidation-dimethylglyoxime photometric method for detecting nickel content in steel - Google Patents
Improved iodine oxidation-dimethylglyoxime photometric method for detecting nickel content in steel Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 96
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 64
- 239000010959 steel Substances 0.000 title claims abstract description 64
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000011630 iodine Substances 0.000 title claims abstract description 35
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 120
- 238000011161 development Methods 0.000 claims abstract description 43
- 238000002835 absorbance Methods 0.000 claims abstract description 31
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000010413 mother solution Substances 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- 239000002253 acid Substances 0.000 claims description 36
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 238000005375 photometry Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000012085 test solution Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000010941 cobalt Substances 0.000 description 7
- 229910017052 cobalt Inorganic materials 0.000 description 7
- 230000006641 stabilisation Effects 0.000 description 7
- 238000011105 stabilization Methods 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000011481 absorbance measurement Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- -1 ammonium citrate dimethylglyoxime Chemical compound 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- UPDATVKGFTVGQJ-UHFFFAOYSA-N sodium;azane Chemical compound N.[Na+] UPDATVKGFTVGQJ-UHFFFAOYSA-N 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000805 Pig iron Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011981 development test Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses an improved iodoxidation-dimethylglyoxime photometric method for detecting nickel content in steel, which comprises the steps of carrying out acidolysis on nickel-containing steel to be detected to obtain acidolysis solution, and then diluting to obtain mother solution to be detected; mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development liquid to be detected; and placing the color development solution to be tested below the critical temperature to carry out photometric test to obtain the nickel content in the nickel-containing steel to be tested. According to the invention, the stability time of the absorbance of the solution to be detected is more than or equal to 60 minutes by controlling the addition amount of ammonium citrate and dimethylglyoxime in the solution to be detected, the detection result of the nickel content in steel with the copper content of less than or equal to 0.2 percent and the nickel content of 0.10 to 50 percent exceeds the probability of the difference of the navigation mark tolerance of less than or equal to 5 percent.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to an improved iodoxidation-dimethylglyoxime photometric method for detecting the content of nickel in steel.
Background
The dimethylglyoxime photometry for detecting the nickel content in the steel comprises a sodium (ammonium) persulfate oxidation-dimethylglyoxime photometry and an iodine oxidation-dimethylglyoxime photometry in an ammonia solution. The sodium (ammonium) persulfate oxidation-dimethylglyoxime spectrophotometry has the advantages of low color development speed, high sensitivity and long absorbance stabilization time, is suitable for detecting the nickel content in copper-containing steel, but is not suitable for detecting the nickel content in high-cobalt steel due to serious interference of cobalt. The iodine oxidation-butanone oxime photometric method in the ammonia solution has high color development speed, completes color development instantly, does not interfere with cobalt, but has low sensitivity, extremely short time for stabilizing absorbance, less than 12 minutes for stabilizing time, and difficult control of field operation, thus leading the detection result to exceed the probability of navigation mark tolerance difference by more than 60 percent.
Research shows that the absorbance stabilization time of the iodine oxidation-butanone oxime photometric method in the ammoniacal solution is related to the adding amount of ammonium citrate dimethylglyoxime in the chromogenic solution to be detected and the chromogenic temperature.
However, no relevant studies have been reported. There is a need to improve the photometric method of iodonium-butanone oxime in ammoniacal solutions, to increase the stabilization time for detecting nickel content in steel and to reduce the probability of exceeding the standard tolerance.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides an improved iodoxidation-dimethylglyoxime photometric method for detecting the content of nickel in steel, which comprises the following steps
Carrying out acidolysis on nickel-containing steel to be detected to obtain acidolysis solution, and then diluting to obtain mother solution to be detected;
mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development liquid to be detected;
and placing the developing solution to be tested below the critical temperature to carry out photometric test to obtain the nickel content in the nickel-containing steel to be tested.
Further, the step of mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development solution to be detected comprises,
and mixing 8-12mL of mother solution to be detected with 15-25mL of ammonium citrate solution, 15-25mL of water, 4-6mL of iodine solution, 8-12mL of ammonia water and 15-25mL of dimethylglyoxime solution to obtain a color development solution to be detected.
Further, the concentration of the ammonium citrate solution is 500g/L.
Further, the iodine solution is a mixed solution of 25.4g/L potassium iodide and 0.1mo/L elemental iodine.
Further, the concentration of the aqueous ammonia was 0.9g/mL.
Further, the concentration of the dimethylglyoxime solution is 2.00g/L.
Further, the critical temperature is 26 ℃.
Further, the copper content in the nickel-containing steel to be detected is less than or equal to 0.2 percent, and the nickel content is 0.10 to 50 percent.
Further, the acidolysis solution obtained by acidolysis of the nickel-containing steel to be tested comprises,
carrying out acidolysis by using different types of acid solutions according to different nickel contents in the nickel-containing steel;
the acid solution comprises concentrated hydrochloric acid, concentrated nitric acid, mixed acid solution of nitric acid, hydrochloric acid and water, mixed acid of nitric acid and hydrochloric acid, and mixed acid of sulfuric acid and phosphoric acid.
Further, the step of placing the color development solution to be tested below critical temperature to perform photometric test to obtain the nickel content in the nickel-containing steel to be tested comprises,
placing the solution to be detected for color development below a critical temperature, standing for 5-10 minutes, and then transferring to a spectrophotometer to detect absorbance at the wavelength of 530 nm;
and calculating according to the absorbance to obtain the nickel content in the nickel-containing steel to be detected.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the stability time of the absorbance of the solution to be detected is more than or equal to 60 minutes by controlling the addition amount of ammonium citrate and dimethylglyoxime in the solution to be detected, the detection result of the nickel content in steel with the copper content of less than or equal to 0.2 percent and the nickel content of 0.10 to 50 percent exceeds the probability of the difference of the navigation mark tolerance of less than or equal to 5 percent.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the steps particularly pointed out in the written description and drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 shows a flow chart of an improved iodoxidation-dimethylglyoxime photometric method for detecting the nickel content in steel according to the invention.
Detailed Description
The iodine oxidation-dimethylglyoxime photometric method for detecting the nickel content in the steel has poor stability, so that the probability of the detection result exceeding the navigation mark allowable difference is more than 60 percent. The invention finds that the addition amounts of ammonium citrate and dimethylglyoxime in the color development solution to be detected and the color development temperature have great influence on the color development stability. By controlling the addition amount of the ammonium citrate and the dimethylglyoxime at a lower color development temperature, the stability time of the absorbance of the color development solution to be detected can be obviously improved so as to reduce the probability of exceeding the allowable difference of the navigation mark.
To this end, as shown in FIG. 1, the present invention provides an improved iodoxidation-dimethylglyoxime photometric method for detecting the nickel content in steel, comprising the steps of,
s101, acidolyzing the nickel-containing steel to be detected to obtain acidolysis solution, and then diluting to obtain mother solution to be detected.
Preferably, the copper content in the nickel-containing steel to be detected is less than or equal to 0.2 percent, and the nickel content is 0.10 to 50 percent.
Preferably, the nickel-containing steel to be tested can be pig iron, iron powder, carbon steel, alloy steel, high-temperature alloy and precision alloy.
Preferably, different kinds of acid liquor are used for acidolysis according to the nickel content of the nickel-containing steel to be detected.
Preferably, the acid solution comprises concentrated hydrochloric acid, concentrated nitric acid, a mixed acid solution of nitric acid, hydrochloric acid and water, a mixed acid of nitric acid and hydrochloric acid, and a mixed acid of sulfuric acid and phosphoric acid.
In the embodiment of the invention, hydrochloric acid with the density of 1.19g/mL, mixed acid liquor of nitric acid with the density of 1.42g/mL and water or mixed acid of hydrochloric acid with the density of 1.19g/mL and nitric acid with the density of 1.42g/mL is used for acidolysis of the nickel-containing steel to be detected, wherein the volume ratio of hydrochloric acid, nitric acid and water in the mixed acid liquor is different, and different types of mixed acid liquor are selected according to different contents of tungsten, molybdenum and niobium in the nickel-containing steel to be detected.
Preferably, the acid solution comprises a first mixed acid, a second mixed acid, a third mixed acid, a fourth mixed acid, a fifth mixed acid and a sixth mixed acid, wherein the first mixed acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL, nitric acid with the density of 1.42g/mL and water in a volume ratio of 3:2:5, mixing the components; the second mixed acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL, nitric acid with the density of 1.42g/mL and water in a volume ratio of 1:4:4, mixing; the third mixed acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL, nitric acid with the density of 1.42g/mL and water in a volume ratio of 1:12:1, mixing; the fourth mixed acid is nitric acid (1 + 3); the fifth mixed acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL and nitric acid with the density of 1.42g/mL according to the volume ratio of 12:1, mixing; the sixth mixed acid is prepared by mixing sulfuric acid with the density of 1.84g/mL and phosphoric acid with the density of 1.70g/mL according to the volume ratio of 1:4, mixing the components.
In a preferred embodiment of the present invention, as shown in table 1, according to the difference of nickel content in the nickel-containing steel to be tested, a certain volume of acid solution is used to perform acidolysis on the nickel-containing steel to be tested to obtain acidolysis solution, then the solution is diluted to obtain mother solution to be tested, and then a small portion of the mother solution to be tested is taken to perform the subsequent absorbance test.
TABLE 1 selection of parameters for acidolysis of nickel-containing steels to be tested
When the to-be-measured nickel-containing steel is subjected to acidolysis by using a mixed acid of hydrochloric acid having a density of 1.19g/mL and nitric acid having a density of 1.42g/mL, the ratio of the hydrochloric acid having a density of 1.19g/mL to the nitric acid having a density of 1.42g/mL can be appropriately adjusted to ensure that the to-be-measured nickel-containing steel sample is completely dissolved.
In the embodiment of the invention, if the nickel-containing steel to be tested is a high-tungsten sample, 0.1-0.2g of the high-tungsten sample is dissolved by using 100-120mL of fifth mixed acid, 10mL of sixth mixed acid is added and mixed uniformly, 25mL of nitric acid with the density of 1.42g/mL is added, then the mixture is heated until smoke of sulfur and phosphoric acid is emitted, the mixture is cooled to room temperature, 50mL of water is added, 10mL of hydrochloric acid with the density of 1.19g/mL is added, the mixture is heated to boiling after being mixed uniformly, and the mixture is diluted to 500mL after being cooled to room temperature to obtain the mother solution to be tested.
In the invention, hydrochloric acid with the density of 1.19g/mL, nitric acid with the density of 1.42g/mL, sulfuric acid with the density of 1.84g/mL and phosphoric acid with the density of 1.70g/mL are common concentrated hydrochloric acid, concentrated nitric acid, concentrated sulfuric acid and phosphoric acid.
And S102, mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development liquid to be detected.
In the embodiment of the invention, 8-12mL of mother solution to be detected, 15-25mL of ammonium citrate solution, 15-25mL of water, 4-6mL of iodine solution, 8-12mL of ammonia water and 15-25mL of dimethylglyoxime solution are mixed to obtain the color development solution to be detected.
Preferably, the concentration of the ammonium citrate solution is 500g/L.
Preferably, the iodine solution is a mixed solution of 25.4g/L potassium iodide and 0.1mo/L elemental iodine. The preparation method of the iodine solution can be that 25.4g of potassium iodide and 12.7 elementary iodine are weighed in a 250 or 300mL wide-mouth beaker, 100-150mL of water is added, the mixture is completely dissolved by stirring, and the mixture is transferred to a 1000mL volumetric flask to be constant in volume with water and then mixed uniformly to obtain the iodine solution.
Preferably, the concentration of the ammonia water is 0.9g/mL.
Preferably, the concentration of the dimethylglyoxime solution is 2.00g/L. The preparation method of the dimethylglyoxime solution can be that 500mL of water, 20g of sodium hydroxide and 4.00 g of dimethylglyoxime are added into a 1000mL wide-mouth plastic beaker, stirred and dissolved completely, transferred to a 2000mL volumetric flask, added with water to a constant volume and mixed uniformly to obtain the dimethylglyoxime solution.
Preferably, multiple groups of the developing solutions to be detected are prepared in parallel, and the average value of absorbance is calculated.
In the embodiment of the invention, cobalt consumes iodine to influence the color development effect, the cobalt content in the transfer solution is controlled to be not more than 40mg, and when the cobalt content in the transfer solution is more than 5mg and not more than 40mg, the cobalt content of the transfer solution is increased by dividing 5.893 of iodine solution.
S103, placing the color development solution to be tested below a critical temperature to perform a photometric method test to obtain the nickel content in the nickel-containing steel to be tested.
Preferably, the critical temperature is 26 ℃.
More preferably, the critical temperature is 25 ℃, the developing temperature of the developing solution to be tested is controlled to be less than or equal to 25 ℃, and when the temperature is higher than 25 ℃, the developing solution to be tested can be transferred to an air-conditioning chamber with the temperature of less than or equal to 25 ℃ for developing and then the subsequent test is completed.
Preferably, the solution to be detected is placed below the critical temperature and is kept still for 5-10 minutes, and then the solution is transferred to a spectrophotometer to detect the absorbance at the wavelength of 530 nm; and calculating according to the absorbance to obtain the nickel content in the nickel-containing steel.
Preferably, the reference solution used in detecting absorbance is water.
In the embodiment mode of the invention, after the color development solution to be detected is kept stand at the temperature of less than or equal to 26 ℃ for 5-10 minutes, a part of the absorption solution is transferred to a cuvette and placed on a 722-type visible spectrophotometer, and the absorbance detection is carried out by taking a solution prepared by completely the same operation as the color development solution as a reference solution without adding the dimethylglyoxime solution. The standard curve is established by methods commonly used in the art: weighing 4-6 parts of standard sample, controlling the nickel content of the weighed sample to be detected within the nickel content range of the standard sample, measuring a series of absorbances according to the operation of the analysis steps, and performing linear regression on the nickel content of the standard sample to the corresponding absorbances to obtain a working curve function. The relationship between the color development temperature and the absorbance stabilization time is shown in Table 2.
TABLE 2 relationship between color development temperature and absorbance stabilization time
As can be seen from the results in Table 2, the method controls the addition amount of the ammonium citrate, the iodine solution and the dimethylglyoxime in the solution to be tested for color development, controls the color development temperature to be less than or equal to 26 ℃, and improves the absorbance stabilization time of the nickel content test to be more than 60 minutes. Meanwhile, the lower the temperature in the color development test, the longer the absorbance stabilization time.
Based on the results of table 2, the present invention gives guidance on the development temperature and the recommended detection time: the developing temperature is 22.5-25 ℃, and the absorbance measurement is completed within 60 minutes after the development; the developing temperature is 20.0-22.5 ℃, and the absorbance measurement is completed within 90 minutes after the development; the developing temperature is 15-20 ℃, and the absorbance measurement is completed within 120 minutes after developing; the development temperature was <15 ℃ and the absorbance measurement was completed within 180 minutes after development.
Preferably, the nickel content in the nickel-containing steel to be measured is calculated according to the following formula:
in the formula, W Ni M is the nickel content in the nickel-containing steel to be measured 0 And m is the quality of the nickel-containing steel to be measured, wherein the measured absorbance is calculated according to the working curve function.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Examples
This example applies the improved iodoxidation-dimethylglyoxime photometric method for detecting the nickel content in steel of the invention to the test of the nickel content in a standard sample. The specific process of obtaining the mother liquor by acidolysis dilution, the process of establishing the work curve function, and the like are not described in detail. The method comprises the following steps:
step 1, performing acidolysis on standard nickel-containing steel to be detected to obtain acidolysis solution, and then diluting to obtain mother solution to be detected;
step 2, testing and mixing 10mL of mother solution to be tested, 20mL of 500g/L ammonium citrate solution, 20mL of water, 5mL of iodine solution (a mixed solution of 25.4g/L potassium iodide and 0.1mol/L elemental iodine), 10mL of ammonia water with the concentration of 0.9g/mL and 20mL of 2.00g/L dimethylglyoxime solution to obtain a color development solution to be tested;
and 3, standing the color development solution to be detected at 25 ℃ for 5 minutes for color development, transferring a small amount of the color development solution to be detected after color development to a cuvette, loading the color development solution to a 722 type visible spectrophotometer, and carrying out absorbance detection by taking a solution prepared by completely the same operation as the color development solution without adding the dimethylglyoxime solution as a reference solution. And (3) testing the absorbance at the wavelength of 530nm, and calculating the nickel mass in the standard sample according to the absorbance and the working curve function so as to obtain the nickel content in the standard sample.
The results of the nickel content test of a series of standard samples are shown in table 3, wherein the absorbance stability time of the developing solution to be tested exceeds 70 minutes for the standard samples in the table, and the absorbance test within 60 minutes is recommended to be suitable.
TABLE 3 test results for nickel content of standard samples
As can be seen from the test results in Table 3, the improved method for detecting nickel content in steel according to the present embodiment has a nickel content detection value in the iodine oxidation-dimethylglyoxime photometric method which is very close to a nickel content standard value, and the allowable difference probability of exceeding the navigation mark is less than 5%.
Comparative example
In the conventional iodine oxidation-dimethylglyoxime photometric method for detecting the nickel content in steel, because the developing temperature and the control range of divalent copper of the developing solution are not specified, and the adding concentration of ammonium citrate and dimethylglyoxime in the developing solution is half of the adding concentration of the invention, the stability is poor: the absorbance of the developing solution is stable for 10-20 minutes at the room temperature of less than 15 ℃, is stable for 5-10 minutes at the room temperature of 15-25 ℃, and is stable for 5 minutes at the room temperature of more than 25 ℃. The absorbance stability of the low color development liquid leads the detection result to exceed the probability of the navigation mark allowable difference by more than 60 percent.
In summary, the method obtains the acidolysis solution by acidolysis of the nickel-containing steel to be detected, and then dilutes the acidolysis solution to obtain the mother solution to be detected; mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development liquid to be detected; and placing the color development solution to be tested below the critical temperature for photometric test to obtain the nickel content in the nickel-containing steel. According to the invention, the stability time of the absorbance of the solution to be detected is more than or equal to 60 minutes by controlling the addition amount of ammonium citrate and dimethylglyoxime in the solution to be detected, the detection result of the nickel content in steel with the copper content of less than or equal to 0.2 percent and the nickel content of 0.10 to 50 percent exceeds the probability of the difference of the navigation mark tolerance of less than or equal to 5 percent.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. An improved iodine oxidation-dimethylglyoxime photometric method for detecting the nickel content in steel is characterized by comprising the following steps,
carrying out acidolysis on nickel-containing steel to be detected to obtain acidolysis solution, and then diluting to obtain mother solution to be detected;
mixing the mother solution to be detected with an ammonium citrate solution, water, an iodine solution, ammonia water and a dimethylglyoxime solution to obtain a color development solution to be detected;
and placing the developing solution to be tested below the critical temperature to carry out photometric test to obtain the nickel content in the nickel-containing steel to be tested.
2. The improved iodine oxidation-dimethylglyoxime photometry for detecting the nickel content in steel as claimed in claim 1, wherein the mixing of the mother liquor to be tested with the ammonium citrate solution, water, the iodine solution, the ammonia water and the dimethylglyoxime solution to obtain the color-developing test solution comprises,
and mixing 8-12mL of mother solution to be detected, 15-25mL of ammonium citrate solution, 15-25mL of water, 4-6mL of iodine solution, 8-12mL of ammonia water and 15-25mL of dimethylglyoxime solution to obtain a color development solution to be detected.
3. The improved iodoxidation-dimethylglyoxime photometric method for detecting the nickel content of steel according to claim 2 wherein the concentration of the ammonium citrate solution is 500g/L.
4. The improved iodoxidation-dimethylglyoxime photometric method for the determination of the nickel content of steel according to claim 2 wherein the iodine solution is a mixed solution of 25.4g/L potassium iodide and 0.1mo/L elemental iodine.
5. The improved iodoxidation-dimethylglyoxime photometric method for the detection of the nickel content of steel according to claim 2 wherein the ammonia is present in a concentration of 0.9g/mL.
6. The improved iodoxidation-dimethylglyoxime photometric method for the detection of the nickel content of steel according to claim 2 wherein the dimethylglyoxime solution has a concentration of 2.00g/L.
7. The improved iodoxidation-dimethylglyoxime photometry for the detection of the nickel content in steel as claimed in claim 1, characterized in that the critical temperature is 26 ℃.
8. The improved iodine oxidation-dimethylglyoxime photometric method for detecting the nickel content in steel according to any one of claims 1 to 7, characterized in that the copper content in the steel containing nickel to be detected is less than or equal to 0.2 percent and the nickel content is 0.10 to 50 percent.
9. The improved iodoxidation-dimethylglyoxime photometry for detecting the nickel content in steel as claimed in claim 8, wherein the acidolysis of the nickel-containing steel to be detected to obtain an acidolysis solution comprises,
performing acidolysis by using different types of acid liquor according to different nickel contents in the nickel-containing steel;
the acid solution comprises concentrated hydrochloric acid, concentrated nitric acid, mixed acid solution of nitric acid, hydrochloric acid and water, mixed acid of nitric acid and hydrochloric acid, and mixed acid of sulfuric acid and phosphoric acid.
10. The improved iodoxidation-dimethylglyoxime photometric method for detecting nickel content in steel as defined in claim 1 wherein the photometric test of the chromogenic solution to be tested at a temperature below the critical temperature to obtain the nickel content in the steel to be tested comprises,
placing the solution to be detected for color development below a critical temperature, standing for 5-10 minutes, and then transferring to a spectrophotometer to detect absorbance at the wavelength of 530 nm;
and calculating according to the absorbance to obtain the nickel content in the nickel-containing steel to be detected.
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