CN106053458A - Method for determining phosphorus content in phosphating solution - Google Patents
Method for determining phosphorus content in phosphating solution Download PDFInfo
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- CN106053458A CN106053458A CN201610517135.4A CN201610517135A CN106053458A CN 106053458 A CN106053458 A CN 106053458A CN 201610517135 A CN201610517135 A CN 201610517135A CN 106053458 A CN106053458 A CN 106053458A
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- phosphating solution
- phosphorus
- determining
- solution
- absorbance
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000011574 phosphorus Substances 0.000 title claims abstract description 37
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 42
- 238000002835 absorbance Methods 0.000 claims abstract description 16
- 239000012086 standard solution Substances 0.000 claims abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 6
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 6
- 230000008030 elimination Effects 0.000 claims abstract description 4
- 238000003379 elimination reaction Methods 0.000 claims abstract description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 7
- 238000003556 assay Methods 0.000 claims description 7
- 229940005654 nitrite ion Drugs 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 5
- 239000012916 chromogenic reagent Substances 0.000 claims description 3
- PMUIBVMKQVKHBE-UHFFFAOYSA-N [S].NC(N)=O Chemical compound [S].NC(N)=O PMUIBVMKQVKHBE-UHFFFAOYSA-N 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 abstract description 6
- -1 nitrite ions Chemical class 0.000 abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 abstract 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- OTGFEQJKSRFOED-UHFFFAOYSA-N [P].[V].[Mo] Chemical compound [P].[V].[Mo] OTGFEQJKSRFOED-UHFFFAOYSA-N 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-M chlorate Inorganic materials [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005406 washing 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention relates to a method for determining phosphorus content in a phosphating solution, and solves the problems that an existing measuring method is large in error of a determining result and long in analysis period and other ingredients disturb the determining method. The method comprises the following steps: elimination of disturbance: in order to eliminate disturbance of the color, determining absorbance by using the phosphating solution as a blank, determining absorbance of color developing liquid by using short wavelength, and selecting the wavelength range to be between 260 nm-315 nm; eliminating disturbance of nitrite ions by using thiourea or sulfamic acid; preparing a phosphorus standard solution by using a standard monopotassium phosphate reagent, selecting a series of standard solutions with different contents, adding a color developing agent under a certain acidity condition to develop color, and measuring the absorbance on a spectrophotometer; drawing of a working curve: developing color and determining the phosphating solution by the same operation, finding out the phosphorus content on the working curve, and calculating to obtain the phosphorus content in the phosphating solution. The method is accurate in analysis result and high in detection efficiency.
Description
Technical field:
The present invention relates to a kind of chemical composition analysis method, be specifically related to the assay method of phosphorus content in a kind of Phosphating Solution.
Background technology:
Phosphating Solution complicated component, although different types of Phosphating Solution composition is different, but is mainly all by phosphate, di(2-ethylhexyl)phosphate
Hydrogen salt, free acid, oxidisability accelerator, accelerator, anti-slag chelating agent etc. form.Substantially contain Zn2+、Mn2+、Cu2+、Ni2+Deng
The aniones such as metal ion and nitrate anion, nitrite anions, chlorate anions and citric acid, tartaric acid, sodium molybdate etc..Phosphating Solution mainly by
Control the total acidity regulation solution of solution, then it is the most qualified to observe film by engineer testing, determines whether solution meets the requirements.This
Plant tank liquor to control to belong to extensive monitor mode.Regulate solution by adding acid ingredient, whether ignore other composition in control
In the range of system, it is extremely difficult to quality control requirement.Sometimes require that in mensuration Phosphating Solution, whether other component content determines Phosphating Solution
Meeting the requirements, wherein the mensuration of phosphorus content is one of them.
Phosphorus yield in Phosphating Solution, usual way is to titrate with standard solution of sodium hydroxide, indicates by indicator
Terminal, is converted by acidity and calculates the content of phosphorus, owing to there is nitrate, phosphate, dihydric phosphate, Fructus Citri Limoniae in Phosphating Solution
Hydrochlorate, phosphatization additive etc., these materials mix and there is complicated hydrolysis and complexation equilibrium, the end of indicator instruction
Point, is difficult to judge, this method error is big.Have been reported that with phosphorus molybdenum acid ammonium capacity method be measured (" plating and finish ", 2012
8th phase, 41-43, Liu Zhiyong, gold are joyous), this method first becomes phosphorus into ammonium phosphomolybdate precipitation, then precipitation is filtered, washing,
Being measured by acid-base titrations after dissolving, analytical cycle is long.Still an alternative is that ammoniomagnesium phosphate gravimetric method, this method needs
Carrying out in ammonium solution, metal ion easily forms precipitation, interference measurement.
Summary of the invention:
The present invention, by providing a kind of method of phosphorus content in phosphorus vanadium molybdenum Huang spectrophotometry Phosphating Solution, solves at present
In measuring method, in Phosphating Solution, phosphorus yield resultant error is big, the shortcoming of analytical cycle length, solves in Phosphating Solution other simultaneously
The problem that assay method is disturbed by composition.
The present invention is realized by techniques below scheme:
The assay method of phosphorus content in a kind of Phosphating Solution, comprises the following steps:
1) elimination disturbed: the interference of color, first originally carries out the mensuration of absorbance, then uses short with Phosphating Solution as blank
Wavelength measures the absorbance of nitrite ion, and wave-length coverage is selected between 260nm～315nm；The interference of nitrite ion,
Eliminate with thiourea or sulfamic acid；
2) becoming phosphorus standard solution with the potassium dihydrogen phosphate preparation of reagents of benchmark, the standard choosing a series of different content is molten
Liquid, adds chromogenic reagent under certain acidity condition, measures its absorbance, drawing curve on spectrophotometer:
3) Phosphating Solution is carried out developing the color, measuring by identical operation, working curve is found the content of phosphorus, by calculating
Obtain the content of phosphorus in Phosphating Solution.
Beneficial effect: the present invention has the following advantages
The invention provides a kind of accurately, determine quantitative analysis method, it is adaptable to the mensuration of phosphorus content in Phosphating Solution.Its advantage
It is: method is simple, quick, analysis result is accurate, and detection efficiency is high, analysis cost is low, adds phosphorus yield in Phosphating Solution
The selectivity of method.
Detailed description of the invention:
The present invention is the assay method of phosphorus content in a kind of Phosphating Solution, with in phosphorus vanadium molybdenum Huang spectrophotometry Phosphating Solution
The content of phosphorus, comprises the following steps:
1, the elimination of interference:
(1) interference of color: Phosphating Solution itself has color, some is the hydrate such as Cu of nonferrous metal ion2+、Ni2+
Deng, some is other organic component, and this color can disturb the mensuration of absorbance.The way used is: first uses Phosphating Solution
This carries out the mensuration of absorbance as blank, so can eliminate the anti-slag chelating agent such as color and citric acid and survey given wavelength
Absorb；Two is to use short wavelength to measure the absorbance of nitrite ion, wave-length coverage is selected between 260nm～315nm, so
Nitrate ion in Phosphating Solution can also be eliminated disturb in the absorption of ultraviolet region simultaneously.
(2) interference of nitrite ion: nitrite ion has certain reproducibility, has certain doing to measuring
Disturb, eliminate with thiourea or sulfamic acid.
2, becoming phosphorus standard solution with the potassium dihydrogen phosphate preparation of reagents of benchmark, the standard choosing a series of different content is molten
Liquid, adds chromogenic reagent under certain acidity condition, measures its absorbance, drawing curve on spectrophotometer.
3, Phosphating Solution is carried out developing the color, measuring by identical operation, working curve is found the content of phosphorus, by calculating
Obtain the content of phosphorus in Phosphating Solution.
Embodiment:
As a example by nigrescent phosphatizing solution, measuring the content of wherein phosphorus, method includes analyzing the preparation of sample, the joining of standard solution
System, the selection of analysis condition, the drafting of working curve and the mensuration of sample, instrument and reagent: T6 UV, visible light light splitting light
Degree meter；Potassium dihydrogen phosphate standard reagent.
1, the preparation of sample is analyzed: the preparation of assay sample: measure 20mL Phosphating Solution in 100 volumetric flasks, dilute with water
Release to scale, shake up.
2, the preparation of standard sample: weigh 0.4363g potassium dihydrogen phosphate standard reagent (the most in an oven in 105 DEG C of bakings
Dry 2 hours) it is dissolved in 100mL water, move in 200mL volumetric flask, be diluted to scale with water, shake up, this solution every milliliter contains 500
Microgram phosphorus (P)
3, the drafting of working curve: accurately divide with pipet take 0.00,1.00,2.00,4.00,6.00,8.00mL phosphorus mark
Quasi-solution in 100mL volumetric flask, 0.2mL sulfamic acid (1%), add 20mL nitric acid (1+5), 10mL ammonium vanadate
(0.25%), 20mL ammonium molybdate (0.5%), be diluted to scale with water, place 5～10 minutes.
Blank solution: draw 10mL test solution in 100mL volumetric flask, 0.2mL sulfamic acid (1%), be diluted with water to carve
Degree, shakes up.
On spectrophotometer, at 275nm wavelength, measure absorbance, with phosphorus content to absorbance drawing curve.
4, the mensuration of sample: with pipette, extract 10.00mL sample solution in 100mL volumetric flask, 0.2mL sulfamic acid
(1%), shake, add 10mL ammonium vanadate (0.25%), 20mL ammonium molybdate (0.5%), be diluted to scale with water, place 5～10 points
Clock.On spectrophotometer, at 275nm wavelength, measure the absorbance of sample solution.Working curve is found corresponding phosphorus contain
Amount.
5, the calculating of analysis result:
The phosphorus content found on working curve is scaled the content of phosphorus in sample, and computing formula is as follows
In formula:
W (P)---the content g/L of phosphorus in-sample
The quality (g) of the phosphorus found on m-----curve
V-----sample solution divides the volume (L) taken.
Claims (1)
1. an assay method for phosphorus content in Phosphating Solution, is characterized in that: comprise the following steps:
1) elimination disturbed: the interference of color, first originally carries out the mensuration of absorbance, then uses short wavelength with Phosphating Solution as blank
Measure the absorbance of nitrite ion, wave-length coverage is selected between 260nm～315nm；The interference of nitrite ion, uses sulfur
Urea or sulfamic acid eliminate；
2) become phosphorus standard solution with the potassium dihydrogen phosphate preparation of reagents of benchmark, choose the standard solution of a series of different content,
Add chromogenic reagent under certain acidity condition, spectrophotometer measured its absorbance, drawing curve:
3) Phosphating Solution is carried out developing the color, measuring by identical operation, working curve is found the content of phosphorus, is obtained by calculating
The content of phosphorus in Phosphating Solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610517135.4A CN106053458A (en) | 2016-06-29 | 2016-06-29 | Method for determining phosphorus content in phosphating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610517135.4A CN106053458A (en) | 2016-06-29 | 2016-06-29 | Method for determining phosphorus content in phosphating solution |
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| Publication Number | Publication Date |
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| CN106053458A true CN106053458A (en) | 2016-10-26 |
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ID=57200850
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| CN201610517135.4A Pending CN106053458A (en) | 2016-06-29 | 2016-06-29 | Method for determining phosphorus content in phosphating solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106769949A (en) * | 2017-02-22 | 2017-05-31 | 武汉大学 | Optofluidic detector based on phosphorus content in vanadium molybdenum Huang spectrophotometry seawater |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
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| CN101984342A (en) * | 2010-11-01 | 2011-03-09 | 中国一拖集团有限公司 | Method for measuring content of sodium nitrite in water base metal cleaner |
| CN102879345A (en) * | 2012-09-26 | 2013-01-16 | 攀钢集团江油长城特殊钢有限公司 | Method for determining phosphorus content of silicon ferrovanadium |
| CN103398963A (en) * | 2013-08-12 | 2013-11-20 | 攀枝花学院 | Method for analyzing phosphorus in silicon iron |
-
2016
- 2016-06-29 CN CN201610517135.4A patent/CN106053458A/en active Pending
Patent Citations (3)
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| CN101984342A (en) * | 2010-11-01 | 2011-03-09 | 中国一拖集团有限公司 | Method for measuring content of sodium nitrite in water base metal cleaner |
| CN102879345A (en) * | 2012-09-26 | 2013-01-16 | 攀钢集团江油长城特殊钢有限公司 | Method for determining phosphorus content of silicon ferrovanadium |
| CN103398963A (en) * | 2013-08-12 | 2013-11-20 | 攀枝花学院 | Method for analyzing phosphorus in silicon iron |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106769949A (en) * | 2017-02-22 | 2017-05-31 | 武汉大学 | Optofluidic detector based on phosphorus content in vanadium molybdenum Huang spectrophotometry seawater |
| CN109827915A (en) * | 2019-03-12 | 2019-05-31 | 闫宏涛 | A kind of bi-component detection agent measuring phosphorus content |
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