CN105987982A - Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition - Google Patents
Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition Download PDFInfo
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- CN105987982A CN105987982A CN201510084556.8A CN201510084556A CN105987982A CN 105987982 A CN105987982 A CN 105987982A CN 201510084556 A CN201510084556 A CN 201510084556A CN 105987982 A CN105987982 A CN 105987982A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000000203 mixture Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 31
- 238000002835 absorbance Methods 0.000 claims abstract description 26
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 15
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 126
- 235000011007 phosphoric acid Nutrition 0.000 claims description 64
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 29
- 239000011733 molybdenum Substances 0.000 claims description 29
- 229910052750 molybdenum Inorganic materials 0.000 claims description 29
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 13
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 11
- 239000011609 ammonium molybdate Substances 0.000 claims description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims description 11
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical group [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 11
- 150000008107 benzenesulfonic acids Chemical class 0.000 claims description 9
- 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 description 7
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 6
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 6
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical class O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims description 6
- 238000004737 colorimetric analysis Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- BQFYGYJPBUKISI-UHFFFAOYSA-N potassium;oxido(dioxo)vanadium Chemical compound [K+].[O-][V](=O)=O BQFYGYJPBUKISI-UHFFFAOYSA-N 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical compound NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 235000007686 potassium Nutrition 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 125000001424 substituent group Chemical group 0.000 claims description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims 1
- AHIBWURJLGCHAY-UHFFFAOYSA-N [S].C1=CC=CC=C1 Chemical class [S].C1=CC=CC=C1 AHIBWURJLGCHAY-UHFFFAOYSA-N 0.000 claims 1
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 39
- 238000012360 testing method Methods 0.000 description 29
- 239000000843 powder Substances 0.000 description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- 229910019142 PO4 Inorganic materials 0.000 description 10
- 239000010452 phosphate Substances 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 239000011780 sodium chloride Substances 0.000 description 7
- 235000002639 sodium chloride Nutrition 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000012488 sample solution Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000032258 transport Effects 0.000 description 4
- JUSXLWAFYVKNLT-UHFFFAOYSA-N 2-bromobenzenesulfonic acid Chemical group OS(=O)(=O)C1=CC=CC=C1Br JUSXLWAFYVKNLT-UHFFFAOYSA-N 0.000 description 3
- MNURPFVONZPVLA-UHFFFAOYSA-N 2-chlorobenzenesulfonic acid Chemical group OS(=O)(=O)C1=CC=CC=C1Cl MNURPFVONZPVLA-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical class [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 229940092714 benzenesulfonic acid Drugs 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical group OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000012549 training 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
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/182—Specific anions in water
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (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
A composition for measuring orthophosphoric radicals in the water system is prepared from acid in a solid form under environmental conditions, vanadate, molybdate and optional filler, and is used for directly and rapidly measuring orthophosphoric radicals in water without dilution. A method for rapidly measuring orthophosphoric radicals in water without dilution includes the steps of adding the composition into a water sample to form a solution, performing color development, measuring the absorbance of the solution under ultraviolet-visible light, and measuring the concentration of orthophosphoric radicals in water.
Description
Technical field
The present invention relates to a kind of for testing the combination of the solid form of orthophosphoric acid root concentration in water system
Thing, the method using orthophosphoric acid root concentration in said composition measurement water system and use said composition
Measure the purposes of orthophosphoric acid root concentration in water system.
Background of invention
In aqueous industrial system, such as cooling tower and steam kettle, containing the phosphate of orthophosphoric acid root
It is widely used as anticorrosive inhibitor.When as anticorrosive inhibitor, orthophosphoric acid root and material list
Cation on face, such as iron ion and calcium ion, by formed film and protect material surface with
Material surface is avoided to be corroded.But, if orthophosphoric acid root is excessive, it be likely to result in fouling,
Dirty and environmental problem.It is dense that the important goal that water for industrial use processes is intended to control orthophosphoric acid root
Spend in the range of suitably.Accordingly, it would be desirable to often measure orthophosphoric acid root in industrial water system
Concentration.
Existing measurement water system, particularly in water for industrial use in the method for orthophosphoric acid root, common are
Molybdenum yellow method or molybdenum blue method.The first step using molybdenum yellow method and molybdenum blue method is acidified water sample and adds molybdenum
Hydrochlorate, orthophosphoric acid root and molybdate in water sample react in acidic aqueous solution, generate phosphorous molybdenum
The solution of acid (a kind of heteropoly acid).In the second step of molybdenum blue method, to above-mentioned phosphorous molybdic acid
Solution adds reducing agent, such as ascorbic acid, by the bluest for phosphomolybdic acid reduction display.
In molybdenum yellow method, second step is addition developer in the above-mentioned solution containing phosphomolybdic acid, such as
Vanadate is so that solution forms yellow.It follows that utilize spectrophotometer, measure the suction of water sample
Luminosity, by colorimetry, thereby determines that the concentration of orthophosphoric acid root contained in water.Molybdenum blue method is non-
The most sensitive, it is adaptable to measure the orthophosphoric acid root of low concentration.And orthophosphoric acid root in water for industrial use system
Concentration sometimes be up to tens ppm.When in water, the concentration of orthophosphoric acid root is higher, molybdenum blue method
It is easy to saturated, now needs first to be diluted water sample measuring.Compared to molybdenum blue method,
It is relatively wide that molybdenum yellow method measures scope, is more suitable for water for industrial use water sample.
But, in existing molybdenum yellow method, generally use is sulphuric acid or nitric acid etc strong acid
Liquid solution.And the liquid solution of this strong acid is high to the requirement of transport, complex operation, dangerous,
There is certain danger.Additionally, in existing molybdenum yellow method, develop the color and the measurement time be the most long.
It is an object of the invention to the solid form developed a kind of easy transport, be convenient for carrying and use
The compositions in molybdenum yellow method, the water of water for industrial use containing orthophosphoric acid root can be introduced directly into
A step colour developing in system.At the same time, it is desirable to by the detection composition of this solid form, it is possible to quickly
Detect in water system the concentration of contained orthophosphoric acid root, improve detection efficiency.
The test compositions of this solid form, it is possible to long-time storage also keeps stable, will not be right
Environment produces security threat.Use the compositions of this dry powder form in measuring industry water system
Orthophosphoric acid root time, it is easy to prepare, operate safety, simple, low cost, and can be easy
Be used by anyone, even those do not analyze the people of experience.
Invention summary
The present invention relates to a kind of for detecting water system, the particularly group of orthophosphoric acid root in water for industrial use
Compound, the method for the orthophosphoric acid root concentration used in said composition measurement water system and said composition
Purposes.
The invention provides a kind of for measuring the compositions of orthophosphoric acid root concentration in water system, its bag
Contain
The acid of the solid form of (a) 75-98.5 weight %；
The water-soluble molybdenum hydrochlorate of (b) 1-24 weight %；
The developer that phosphomolybdic acid is developed the color of (c) 0.05-1 weight %.
Present invention also offers a kind of for measuring the method for orthophosphoric acid root concentration in water system, its bag
Include the following step:
I () adds the test compositions of the present invention and to formation solution in water sample and develops the color；
(ii) absorbance of described solution is measured.
Present invention also offers in the compositions of the present invention orthophosphoric acid root concentration in measuring water system
Purposes.
Accompanying drawing explanation
Fig. 1 is that absorbance is in time under the 365nm wavelength and 1cm light path of embodiment 1
Change curve.It can be seen that in the concentration range that the present embodiment is suitable for, colour developing can be one
Complete in minute.
Fig. 2 is the absorbance curve to wavelength under the 1cm light path of embodiment 1.
Fig. 3 is that the absorbance under the 380nm wavelength and 1cm light path of embodiment 1 aligns
The calibration trace of phosphate concentration.
Fig. 4 is the absorbance curve to wavelength under the 1cm light path of embodiment 2.
Fig. 5 is the 365nm wavelength in embodiment 2 and the extinction under 1cm optical path length
Degree aligns the calibration trace of phosphate concentration.
Detailed Description Of The Invention
The invention provides a kind of for testing the compositions of orthophosphoric acid root concentration in water system.This
Bright provided compositions is the form of solid form, particularly dry powder doses, it is simple to transports, seal
Dress and use.
In one embodiment of the invention, it is provided that one is used for testing orthophosphoric acid in water system
The compositions of root concentration, comprises the acid of (a) solid form；(b) water-soluble molybdenum hydrochlorate；C () is right
The developer of phosphomolybdic acid colour developing.
Above-mentioned " acid of solid form " refers to be the acid of solid at ambient conditions, wherein " ring
Border condition " represent the temperature and pressure at indoor or outdoors.Preferably, " environmental condition " table
Show the temperature of 16～35 DEG C and the pressure of 1atm.
The acid of this solid form preferably has up to the pKa value of 1.5.It is further preferred that this solid shape
The pKa value of the acid of formula is in the range of-10～1.5；Particularly preferably, the pKa of the acid of this solid form
Value is in the range of-5～1.5.
Preferably, the acid of this solid form is selected from sulfamic acid, benzenesulfonic acid class, trichloroacetic acid and institute
State the mixture of acid.Above-mentioned the mixture of acid " " include two kinds, multiple or all selectable
The mixture of acid.Benzenesulfonic acid class therein includes substituted benzenesulfonic acid, substituent group selected from methyl,
C1～the C4 alkyl of ethyl, propyl group or butyl and selected from chlorine, bromine, the halogen of iodine.This is substituted
Benzenesulfonic acid includes o-C1～C4-alkyl benzene sulphonate, m-C1～C4-alkyl benzene sulphonate, p-C1～C4-
Alkyl benzene sulphonate, adjacent chlorobenzenesulfonic acid, a chlorobenzenesulfonic acid, to chlorobenzenesulfonic acid, adjacent bromo
Benzenesulfonic acid, a bromophenylsulfonic acid, to bromophenylsulfonic acid and and mixture.Preferably, to toluene
Sulfonic acid.
The consumption of the acid of the solid form in the present invention is 75-98.5 weight %；Preferably
78%-98 weight %, more preferably 80%-97.5 weight %.
Water-soluble molybdenum hydrochlorate for the present invention is under acid condition of the present invention, it is possible to
The molybdate forming phosphomolybdic acid is reacted with orthophosphoric acid root.Molybdate in the present invention includes leading to
Those molybdates being commonly used in molybdenum yellow method.Preferably, described molybdate is ammonium molybdate, sodium molybdate
Or potassium molybdate.Those skilled in the art can determine described molybdate according to prior art.
The consumption of the molybdate in the present invention is 1-24 weight %, preferably 2-20 weight %,
More preferably 2-18 weight %.
The developer developed the color by phosphomolybdic acid, refers to the molybdenum in acid condition used in molybdenum yellow method
The developer of the phosphomolybdic acid colour developing that the orthophosphoric acid root reaction in hydrochlorate and water system is formed, such as vanadic acid
Salt, preferably ammonium vanadate, vanadic acid sodium, potassium vanadate.
In the present invention, the consumption of vanadate is 0.05-1 weight %, preferably 0.1-0.8 weight %,
More preferably 0.3-0.7 weight %.
In an embodiment of the invention, it is provided that one is used for testing orthophosphoric acid in water system
The compositions of root concentration, including
(a) 75-98.5 weight %；Preferably 78%-98 weight %, more preferably 80%-97.5% consolidates
The acid of bodily form formula；
(b) 1-24 weight %, preferably 2-20 weight %, the water-soluble molybdenum of more preferably 2-18 weight %
Hydrochlorate；
(c) 0.05-1 weight %, preferably 0.1-0.8 weight %, the general of more preferably 0.3-0.7 weight %
The developer of phosphomolybdic acid colour developing.
In one embodiment of the invention, it is provided that one is used for testing orthophosphoric acid in water system
The compositions of root concentration, including
(a) 75-98.5 weight %；Preferably 78%-98 weight %, more preferably 80%-97.5% consolidates
The acid of bodily form formula, selected from sulfamic acid, benzenesulfonic acid class, trichloroacetic acid and the mixture of described acid；
(b) 1-24 weight %, preferably 2-20 weight %, the water-soluble molybdenum of more preferably 2-18 weight %
Hydrochlorate, preferably ammonium molybdate, sodium molybdate, potassium molybdate；
(c) 0.05-1 weight %, preferably 0.1-0.8 weight %, the water of more preferably 0.3-0.7 weight %
Dissolubility vanadate, preferably ammonium vanadate, vanadic acid sodium, potassium vanadate.
In yet another embodiment of the present invention, said composition comprises 80～97.5 weight %
The acid of solid form, such as p-methyl benzenesulfonic acid, 0.4～0.6 vanadate of weight %, such as vanadic acid
Ammonium, 2～20 molybdates of weight %, such as ammonium molybdate.
In order to mix and the convenience of subpackage (encapsulation), the compositions of the present invention can also comprise and fill out
Material, to adjust reagent total amount, thus is beneficial to preparation and subpackage.Such as, when the consumption of compositions
The when of the lowest, the small error produced during subpackage, all may bring the biggest to testing result
Deviation.It is therefore preferable that add filler in the composition, to facilitate preparation and the subpackage of compositions.
This filler can be not affect color in phosphomolybdic acid process color to develop, to the positive phosphorus in water system
Other component in acid group and compositions is inert material, usually sodium chloride, potassium chloride,
Potassium nitrate class inorganic salt.In one embodiment, described inorganic salt is sodium chloride.
The amount of filler, depends on the convenience of preparation, can arbitrarily add, and for example, tests combination
One times of thing weight or several times, as long as it does not affect the measurement aligning phosphate radical, this for
Those skilled in the art are clearly.
In an embodiment of the invention, it is provided that a kind of for testing the positive phosphorus in water system
The dry powder agent composite of acid group concentration, including the acid of (a) solid form, be selected from sulfamic acid,
P-methyl benzenesulfonic acid, trichloroacetic acid and mixture thereof；(b) molybdate；(c) showing for phosphomolybdic acid
Toner, such as vanadate；(d) filler, such as sodium chloride or potassium nitrate.Wherein the amount of filler is
On the basis of original compositions, it is added as needed on, for example, compositions effective ingredient weight
0 times of amount with up to 10 times.
In an embodiment of the invention, said composition comprises the solid of 20～25 weight %
The acid of form, such as sulfamic acid, the vanadate of 0.1～0.2 weight %, such as ammonium vanadate, 4～5
The molybdate of weight %, such as ammonium molybdate and the filler of 70～75 weight %, such as sodium chloride.
In an embodiment of the invention, said composition includes consolidating of (a) 90-97.5 weight %
The acid of bodily form formula, is selected from sulfamic acid, benzenesulfonic acid class, trichloroacetic acid and mixture thereof；
The ammonium molybdate of (b) 2～2.5 weight %；(c) 0.4～0.5 weight % vanadate, such as ammonium vanadate；(d)
The filler of surplus, such as sodium chloride.
It has surprisingly been found that by selecting the acid of solid form, molybdate and the ratio of developer especially
Example, it is possible to realize quick colour-developing such that it is able to detect orthophosphoric acid root in water system more quickly
Concentration.It has been unexpectedly discovered that, adjust the ratio of each component in compositions so that solid form
Acid, vanadate and molybdate (calculating based on the amount of single molybdenum) be dissolved in sample after rub
You are respectively 50-100,0.02-0.06,5-10 mM every liter at concentration, preferably 60-90,
0.03-0.05,6-9 mM every liter, more preferably 70-85,0.032-0.040,6.5-8 mM
When every liter, be conducive to when said composition is added in water sample, make this water sample quick colour-developing, from
And the concentration of the orthophosphoric acid root in water sample can be detected more quickly.Preferably, the combination of the present invention
The acid of solidapowder form in thing, vanadate and molybdate (are carried out based on the amount of single molybdenum
Calculate) mol ratio be 7-13:0.002-0.1:1.
Being used for of the present invention measures water system, the particularly compositions of orthophosphoric acid root in water for industrial use,
It is by the acid of solid form, molybdate, developer and optional filler are mixed to form homogeneous
Dry powder and prepare.
The compositions in dry powder form of the present invention may be used for measuring water system, particularly industry
Concentration with the orthophosphoric acid root in water.During use, water sampling, by direct for described solid composite
Joining in water sample, vibration makes water sample mixing colour developing.Use spectrophotometer, measure water sample
Color, determines the concentration of orthophosphoric acid root in water system according to the color manifested by colorimetry.
Water system alleged in the present invention generally refers to water for industrial use system, and particularly those need really
Determine the water for industrial use system of the concentration of orthophosphoric acid root in water system, such as cooling tower, steam boiler etc.
Water for industrial use system.
In one embodiment of the invention, it is provided that one is used for measuring orthophosphoric acid root in water
The method of concentration, it includes
I () obtains water sample from water for industrial use；
(ii) add to the compositions of the present invention water sample is formed solution and develops the color；
(iii) absorbance of described solution is measured, to determine the concentration of orthophosphoric acid root in described solution.
It is not limited to theory, in the method for the invention, when the compositions of the present invention being added extremely
Time in water sample, orthophosphoric acid root and molybdate react in acid condition, generate phosphomolybdic acid；Described
Phosphomolybdic acid and developer react with colour developing.It follows that use spectrophotometer (tintometer)
At 300～600nm wavelength, preferably 350～450nm wavelength under measure the ultraviolet-visible of water sample and inhale
Luminosity, by colorimetry, such as, utilizes and the standard solution containing orthophosphoric acid root obtained in advance
Absorbance curve (calibration trace) compare, and obtain the dense of the orthophosphoric acid root in water system
Degree.
In order to obtain above-mentioned calibration trace, the body such as grade of different known orthophosphoric acid root concentration will be comprised
Long-pending water sample is placed under ultraviolet-visible analysis, measures the absorbance under each concentration.Then,
The data that will record, draw absorbance and align the curve chart of phosphate concentration, and this curve chart is
Above-mentioned calibration trace.
In the present invention, the orthophosphoric acid root concentration using the compositions of dry powder form to test can be
The water system that orthophosphoric acid radical content is the lowest, the most as little as close to the water system of 0ppm, it is also possible to is just
The water system that phosphate content is higher, the most up to water sample containing 100ppm orthophosphoric acid root.Preferably,
The compositions of the present invention can test orthophosphoric acid radical content such as 0 with up to 80ppm, preferably
0 with up to 50ppm, and more preferably 0 with up to 30ppm, even more preferably from 0 with up to 20ppm's
Water sample.
Preferably, said composition is for 1 milliliter of water sample, to add the compositions of 10～100 milligrams
Ratio add measure to water sample.
Embodiment
The invention is not restricted to following embodiment.Be given following embodiment be intended to illustrate and
It is not intended to limit the scope of the present invention.The scope of the present invention is based on claim.This
Numerical value in bright, unless otherwise defined, is percentage by weight based on compositions gross weight.
Embodiment 1
In this embodiment, 6.35 grams of dry sulfamic acids, the ammonium vanadate of 42 milligrams, 1.27
Gram ammonium molybdate, the sodium chloride of 20 grams grind to form the homogeneous powder of solid of 27.662 grams together.
This powder is uniformly sub-packed in 1000 disposable sacks, each sack comprises about 27.7 millis
Gram this homogeneous powder.The most at ambient conditions, one bag of homogeneous powder is dissolved in the use of 1 milliliter
In the water sample comprising orthophosphoric acid root of test, form water sample to be tested.Water sample is surveyed
The concentration of examination reagent component is listed as follows.
Table 1
| Reagent component | Concentration (the milligram number in one milliliter of water sample) |
| Sulfamic acid | 6.35 |
| Ammonium vanadate | 0.042 |
| Ammonium molybdate | 1.27 |
| Sodium chloride filler | 20.0 |
After the color of water sample changes completely, (using Shimadzu UV-2450 spectrophotometer) is right
Water sample carries out ultraviolet-visible analysis to obtain the absorbance of this sample.Sample is analyzed at ultraviolet-visible
The optical path length that in solution processes, light passes through is 1 centimetre.
Utilize this test compositions, test the orthophosphoric acid root of 30ppm, 10ppm, 1ppm
Concentration.This result is presented in Fig. 1.This sample is monitored by the absorbance under 365nm wavelength
The color change of product solution.Moment 0 refers to that solid test compositions is dissolved completely in water sample also
Moment in mix homogeneously.
From figure 1 it appears that be completely dissolved and from the beginning of mix homogeneously from test agent, one
The color change of sample solution is fully achieved in minute.
Fig. 2 shows in wavelength is 300～600nm and under 1cm optical circuit path, difference is just
The ultraviolet-visible light spectrogram of phosphate concentration.From figure 2 it can be seen that be 350～450 at wavelength
In nm, the absorbance curve to wavelength of variable concentrations can be clearly distinguished.
Fig. 3 is showing in aqueous, the extinction under 380nm wavelength and 1cm optical path length
Degree aligns the calibration trace of phosphate concentration.From figure 3, it can be seen that from 0ppm at least
20ppm, maintains the linear of Absorbance versus concentration curve.The holding of this linear relationship represents
At least when orthophosphoric acid root concentration is in 0～20ppm, and this concentration can be simply by 380nm
Under absorbance be calculated.
Embodiment 2
In this embodiment, p-methyl benzenesulfonic acid is used to replace sulfamic acid.50.64 gram
The ammonium molybdate of p-methyl benzenesulfonic acid, the ammonium vanadate of 0.25 gram and 1.11 grams is mixed together homogeneous, then
Divide equally in 1000 disposable sacks, each sack comprises about 52 milligrams dry molten
The homogeneous powder of agent, at ambient conditions, dissolves the dry homogeneous powder of solvent in each sack
In 1 milliliter of sample water, form sample solution.The component of this homogeneous solvent powder is listed as follows.
Table 2
| Solvent composition | Concentration (the milligram number in one milliliter of water sample) |
| P-methyl benzenesulfonic acid | 50.64 |
| Ammonium vanadate | 0.25 |
| Ammonium molybdate | 1.11 |
When the color of water sample solution has changed, sample solution is carried out ultraviolet-visible analysis use
Obtain the absorbance of this sample.The wavelength of light is analyzed 350～450nm for ultraviolet-visible
In.During ultraviolet-visible analyzes sample solution, the optical path length that ultraviolet-visible light must pass through
Degree is 1 centimetre.
Under the optical path length of 1cm, said composition is for measuring different orthophosphoric acid root concentration.
Fig. 4 is under 350～450nm UV wavelength, the ultraviolet-visible light of different orthophosphoric acid root concentration
Spectrogram.
Fig. 5 shows in this sample, under the wavelength of 365nm and the optical path length of 1cm
Absorbance align the calibration trace of phosphate concentration.
From figure 5 it can be seen that from 0ppm at least 20ppm, maintain absorbance to dense
Write music the linear of line.The holding of this linear relationship represents that at least orthophosphoric acid root concentration is 0～20
In ppm, this concentration can be simply by the absorbance determined under 380nm and calculate
Arrive.
Embodiment 3
The test compositions in embodiment 2 is used to check the repeatability of this test.At 365nm UV
Under the UV, visible light of wavelength is analyzed, two orthophosphoric acid root concentration (2ppm and 20ppm of test respectively
PO4 3-).This test is carried out 17 times, and this result is summarised in table below.
Table 3
| Concentration | Mean light absorbency under 365nm | Standard deviation | Relative standard deviation |
| 2ppm | 0.31 | 0.02 | 6.5% |
| 20ppm | 1.40 | 0.04 | 2.8% |
It can be seen that for low He high orthophosphoric acid root concentration, measure in all of test
Absorbance the most not away from meansigma methods, it is good that this shows in large-scale orthophosphoric acid root concentration
Good detection accuracy.
Embodiment 4
Checked the difference of test compositions own wt to orthophosphoric acid root measurement of concetration in water system
Impact.By 9 test agent powder samples of corresponding embodiment 2, its weight range is from 98～108
Mg, is dissolved separately in 2 milliliters of water samples that (the orthophosphoric acid root concentration in each water sample is one
Cause), it is used for measuring the absorbance under the ultraviolet-visible of 365nm UV wavelength is analyzed.
Table 4
It can be seen that the Light Difference of test composition total weight will not be significantly from above-mentioned table
Affect the measurement of absorbance and the determination of concentration.Therefore, just test composition weight change and
Speech, the concordance of the method is the highest, has reliable sensitivity and accuracy.
Stability study: stability test finds to store at ambient conditions at least 6 months, powder
End does not show any degrades significantly.
Will be apparent from: the powder of present invention test compositions is easily stored, easy to carry and transport,
Easily operated, even in this field not people by professional training can also use.
Additionally, be clear that: above-mentioned method can measure the concentration of orthophosphoric acid root easily, only need
Dry chemical powder compositions and water sample are mixed this step, both need not dilution water sample
Step, it is not required that add molybdate and developer in two steps.Meanwhile, utilize the present invention's
Compositions, it is possible to quick colour-developing, is reduced to tradition molybdenum yellow method developing time from about 7 minutes
1-2 minute, effectively save the detection time, improve detection efficiency.And, use this
Bright compositions, has obtained the highest detection sensitivity and accuracy.
Based on the above, it is understood that: the test compositions of the solid form of the present invention, it is easy to
Store, be easy to carry, conveniently operate.The test compositions of the solid form of the present invention can be quickly
Develop the color, repeated high, there is the sensitivity well tested orthophosphoric acid root in water system with accurate
Property, it is possible to it is effective to measure the concentration of orthophosphoric acid root in water system, particularly water for industrial use, carries
High monitoring efficiency.
Claims (19)
1., for measuring a compositions for orthophosphoric acid root concentration in water system, it comprises
The acid of the solid form of (a) 75-98.5 weight %；
The water-soluble molybdenum hydrochlorate of (b) 1-24 weight %；
The developer that phosphomolybdic acid is developed the color of (c) 0.05-1 weight %.
2. the compositions of claim 1, the acid of wherein said solid form has-10～1.5
PKa value.
3. the compositions of claim 1 or 2, including the solid form of 78-98 weight %
Acid.
4. the compositions any one of claims 1 to 3, including the water of 2-20 weight %
Molybdenum hydrochlorate.
5. the compositions according to any one of Claims 1-4, including 0.1-0.8 weight %
Developer.
6. the compositions of claim 5, wherein developer is vanadate.
7. the compositions any one of claim 1 to 6, the wherein acid of solid form: vanadic acid
Salt: the mol ratio of molybdate is 7-13:0.002-0.1:1, counts based on the amount of single molybdenum
Calculate.
8. the compositions according to any one of claim 1 to 7, wherein said acid is selected from amino
Sulfonic acid, benzenesulfonic acid class, trichloroacetic acid and mixture thereof.
9. the compositions described in claim 8, wherein said benzenesulfonic acid class is substituted benzene sulphur
Acid, wherein said substituent group is selected from C1～C4 alkyl and halogen.
10. the compositions described in claim 8, wherein said acid is p-methyl benzenesulfonic acid or three chloroethenes
Acid.
Compositions according to any one of 11. claim 1 to 10, wherein said molybdate is
Ammonium molybdate, sodium molybdate, potassium molybdate.
Compositions described in 12. claim 6, wherein said vanadate is ammonium vanadate.
Compositions according to any one of 13. claim 1 to 12, the most also includes filler.
Compositions according to any one of 14. claim 1 to 13, including
The acid of the solid form of (a) 80-97.5 weight %, be preferably selected from sulfamic acid, benzenesulfonic acid class,
Trichloroacetic acid and mixture thereof；
The molybdate of (b) 2～20 weight %, preferably ammonium molybdate；
C () 0.1～0.8 weight % vanadate, is preferably selected from ammonium vanadate, vanadic acid sodium, potassium vanadate；
The filler of (d) surplus.
The compositions of 15. claim 14, wherein said vanadate is ammonium vanadate.
16. 1 kinds are used for measuring the method for orthophosphoric acid root concentration in water system, and it comprises the steps:
(i) water sampling,
(ii) compositions according to any one of claim 1 to 15 is joined in water sample and formed
Solution also develops the color；With
(iii) absorbance of described solution is measured.
17. methods according to claim 16, the most also comprise the following steps
(iv) absorbance curve of standard solution containing orthophosphoric acid root is obtained；With
V () passes through the absorbance of colorimetry, absorbance step (iii) measured and standard solution
Curve comparison, to determine the concentration of orthophosphoric acid root in water system.
18. methods according to claim 16, wherein said compositions is with every milliliter of institute
The water sample stated, the ratio of corresponding 10～100 milligrams of described compositionss adds.
The orthophosphoric acid root in measuring water system of the compositions any one of 19. claim 1 to 15 is dense
The purposes of degree.
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| CN201510084556.8A CN105987982A (en) | 2015-02-16 | 2015-02-16 | Composition for measuring concentration of orthophosphoric radicals in water system, measuring method and application of composition |
| PCT/US2016/018031 WO2016133882A1 (en) | 2015-02-16 | 2016-02-16 | Composition and method for measuring orthophosphate concentration in water system and use of said composition |
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| CN109142621A (en) * | 2018-08-21 | 2019-01-04 | 深圳市长隆科技有限公司 | Fast check reagent box of phosphorus and preparation method thereof and phosphorus detection method |
| US10358363B2 (en) | 2015-03-17 | 2019-07-23 | Ecolab Usa Inc. | Fluorescent polymers for water treatment |
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| CN109374615A (en) * | 2018-11-28 | 2019-02-22 | 河北四通新型金属材料股份有限公司 | The analyzing detecting method of molybdenum element in a kind of molybdenum vanadium aluminium intermediate alloy |
| CN113740328B (en) * | 2021-03-08 | 2023-05-02 | 中国科学院物理研究所 | Method for detecting transition metal dissolution amount of secondary battery electrode material and color developing agent |
| EP4286833A1 (en) | 2022-06-01 | 2023-12-06 | Hach Lange GmbH | Methods of determining phosphate concentration in a water sample |
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