CN108107012A - A kind of test reagent combination of total phosphorus in-line analyzer and its method for measuring total phosphorus content in water sample - Google Patents
A kind of test reagent combination of total phosphorus in-line analyzer and its method for measuring total phosphorus content in water sample Download PDFInfo
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- CN108107012A CN108107012A CN201810158353.2A CN201810158353A CN108107012A CN 108107012 A CN108107012 A CN 108107012A CN 201810158353 A CN201810158353 A CN 201810158353A CN 108107012 A CN108107012 A CN 108107012A
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 271
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 134
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 134
- 239000011574 phosphorus Substances 0.000 title claims abstract description 134
- 238000012360 testing method Methods 0.000 title claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 23
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 70
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 51
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 35
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 29
- 235000019394 potassium persulphate Nutrition 0.000 claims abstract description 29
- IIQJBVZYLIIMND-UHFFFAOYSA-J potassium;antimony(3+);2,3-dihydroxybutanedioate Chemical compound [K+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O IIQJBVZYLIIMND-UHFFFAOYSA-J 0.000 claims abstract description 26
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 25
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 25
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 6
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 15
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 12
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 12
- 239000011609 ammonium molybdate Substances 0.000 claims description 12
- 229940010552 ammonium molybdate Drugs 0.000 claims description 12
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 9
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- AUJJPYKPIQVRDH-UHFFFAOYSA-N antimony potassium Chemical compound [K].[Sb] AUJJPYKPIQVRDH-UHFFFAOYSA-N 0.000 claims description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims description 4
- 239000011684 sodium molybdate Substances 0.000 claims description 4
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000003643 water by type Substances 0.000 description 16
- 239000002211 L-ascorbic acid Substances 0.000 description 10
- 235000000069 L-ascorbic acid Nutrition 0.000 description 10
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 9
- 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 description 8
- 238000004458 analytical method Methods 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 229910052708 sodium Inorganic materials 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 238000004939 coking Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009533 lab test Methods 0.000 description 2
- 238000011545 laboratory measurement Methods 0.000 description 2
- 239000010893 paper waste Substances 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- SZXAQBAUDGBVLT-UHFFFAOYSA-H antimony(3+);2,3-dihydroxybutanedioate Chemical compound [Sb+3].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O SZXAQBAUDGBVLT-UHFFFAOYSA-H 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical group [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 235000016768 molybdenum Nutrition 0.000 description 1
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000002133 sample digestion Methods 0.000 description 1
- 230000036413 temperature sense Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
- G01N2001/302—Stain compositions
Abstract
The method that the present invention discloses a kind of test reagent combination of total phosphorus in-line analyzer and its measures total phosphorus content in water sample, wherein, the test reagent combination of the total phosphorus in-line analyzer is suitable for molybdate spectrophotometry, it includes the first reagent, the second reagent and the 3rd reagent, and first reagent contains the potassium peroxydisulfate that concentration is 32.5~40g/L；Second reagent contains the ascorbic acid that concentration is 20~25g/L；3rd reagent contains the molybdate that the concentrated sulfuric acid, concentration that concentration is 100~115mL/L are 22~26g/L and the potassium antimony tartrate that concentration is 0.3~0.4g/L.Technical solution of the present invention provides one kind, and easily storage, stability are good, versatile, can be suitable for the test reagent combination of the total phosphorus automatic analyzer of different brands.
Description
Technical field
The present invention relates to chemical analysis technology field, the test reagent combination of more particularly to a kind of total phosphorus in-line analyzer and
It measures the method for total phosphorus content in water sample.
Background technology
Total phosphorus content assay method includes two kinds of laboratory hand analysis and automatic online analysis in existing water sample；Its
In, the method for total phosphorus content is typically using gravimetric method, titration, spectrophotometry in laboratory hand analysis water-like；It is and total
Phosphorus automatic online analyzer has：Hash Sigma total phosphorus in-line analyzer, HORIBA total phosphorus in-line analyzer, just strange WQ-1000
Total phosphorus in-line analyzer, Shimadzu TNP-4110 total phosphorus in-line analyzers etc..Total phosphorus automatic analyzer is fast with analyze speed, weight
The characteristics of now property is good, and the method for ammonia nitrogen concentration reduces very big workload in opposite manual analyzing water sample, it is domestic present
Progressively start to promote the use of total phosphorus automatic analyzer to measure total phosphorus content in water sample.
But the total phosphorus automatic analyzer of different brands in the prior art, purchase imported with original packaging reagent is generally required, not only
It is expensive, and the additive of imported with original packaging reagent is very sensitive to temperature, it is necessary to it refrigerates.Additive after unlatching is either
No use, expires and fails, and easily causes to waste；And after opening additive, in use in case of several days have a power failure or refrigerator is not made
It is cold, whole bucket reagent is also easily caused to go bad even and is failed.
Therefore, a kind of easily storage is developed, stability is good, versatile, can be suitable for the total phosphorus of different brands certainly
Dynamic analyzer is very necessary.
The content of the invention
The main object of the present invention is to propose a kind of test reagent combination of total phosphorus in-line analyzer, the total phosphorus on-line analysis
The test reagent combination of instrument easily stores, and stability is good, versatile, and the total phosphorus that can be suitable for different brands automatically analyzes
Instrument.
To achieve the above object, the present invention proposes a kind of test reagent combination of total phosphorus in-line analyzer, and it is suitable for molybdenums
Hydrochlorate spectrophotometry, the test reagent combination include the first reagent, the second reagent and the 3rd reagent, and first reagent contains
There is the potassium peroxydisulfate that concentration is 32.5~40g/L；Second reagent contains the ascorbic acid that concentration is 20~25g/L；It is described
3rd reagent contain the concentrated sulfuric acid that concentration is 100~115mL/L, the molybdate that concentration is 22~26g/L and concentration be 0.3~
The potassium antimony tartrate of 0.4g/L.
Preferably, second reagent is also containing the disodium ethylene diamine tetraacetate and concentration that concentration is 0.5~1.5g/L
For the concentrated sulfuric acid of 5~10mL/L.
Preferably, first reagent contains the potassium peroxydisulfate that concentration is 32.5~37.5g/L.
Preferably, second reagent contains the ascorbic acid that concentration is 20~22g/L.
Preferably, the 3rd reagent contains the concentrated sulfuric acid that concentration is 100~110mL/L.
Preferably, the 3rd reagent contains the molybdate that concentration is 22~24g/L.
Preferably, the 3rd reagent contains the potassium antimony tartrate that concentration is 0.3~0.35g/L.
Preferably, the molybdate is ammonium molybdate or sodium molybdate.
The present invention also provides a kind of methods for measuring total phosphorus content in water sample, and this method comprises the following steps：
The aqueous solution containing 32.5~40g/L potassium peroxydisulfates is configured, so as to which the first reagent be made；Configuration contains 20~25g/
The aqueous solution of L ascorbic acid, so as to prepare the second reagent；Configuration contains 100~115mL/L concentrated sulfuric acids, 22~26g/L molybdic acids
The aqueous solution of salt, 0.3~0.4g/L potassium antimony tartrates, so as to prepare the 3rd reagent；By first reagent, second examination
Agent, the 3rd reagent are respectively placed on the precalculated position of total phosphorus in-line analyzer, and water sample is detected, and are measured total in water sample
Phosphorus content.
The test reagent combination for the total phosphorus in-line analyzer that technical solution of the present invention provides, easily storage, stability are good, logical
It is strong with property, the total phosphorus automatic analyzer of different brands can be suitable for.
Specific embodiment
The technical solution in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example is only the part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiments obtained without creative efforts belong to what the present invention protected
Scope.
In addition, the technical solution between each embodiment can be combined with each other, but must be with ordinary skill
Personnel can be implemented as basis, and this technical side is will be understood that when the combination appearance of technical solution is conflicting or can not realize
The combination of case is not present, also not the present invention claims protection domain within.
The present invention proposes a kind of test reagent combination of total phosphorus in-line analyzer and its measures total phosphorus content in water sample
Method.The test reagent combination easily stores, stability is good, versatile, and the total phosphorus that can be suitable for different brands divides automatically
Analyzer, and error is smaller.
The test reagent combination of total phosphorus in-line analyzer proposed by the present invention, it is suitable for molybdate spectrophotometry, institutes
Stating test reagent combination includes the first reagent, the second reagent and the 3rd reagent, first reagent contain concentration for 32.5~
The potassium peroxydisulfate of 40g/L；Second reagent contains the ascorbic acid that concentration is 20~25g/L；3rd reagent contains dense
Spend the concentrated sulfuric acid for 184~211.6g/L, the molybdate that concentration is 22~26g/L and the winestone that concentration is 0.3~0.4g/L
Sour antimony potassium.
Wherein, molybdate spectrophotometry surveys the principle of phosphorus content：Make sample digestion with potassium peroxydisulfate, sample institute is phosphorous
Orthophosphates all is oxidized to, in acid medium, it is miscellaneous more to generate phosphorus molybdenum in the presence of antimonic salt for orthophosphates and molybdic acid reactant salt
It after acid, is reduced immediately by ascorbic acid, generates the complex compound of blueness.Specifically, first reagent mainly plays resolution,
Second reagent mainly plays reduction, and the 3rd reagent mainly plays coloration.
Preferably, first reagent contains the potassium peroxydisulfate that concentration is 32.5~37.5g/L；Second reagent contains
Concentration is the ascorbic acid of 20~22g/L；3rd reagent contains the concentrated sulfuric acid that concentration is 100~110mL/L；Described 3rd
Reagent contains the molybdate that concentration is 22~24g/L；3rd reagent contains the antimony tartrate that concentration is 0.3~0.35g/L
Potassium.It should be noted that the density of the concentrated sulfuric acid is 1.84g/mL.The molybdate can be ammonium molybdate or sodium molybdate.
The imported with original packaging reagent of the total phosphorus in-line analyzer of the prior art, it is not only expensive but also very quick to temperature
Sense, the shelf-life is shorter, general only 1 month.In order to improve the test reagent combination of total phosphorus in-line analyzer provided by the invention
Shelf-life, prolong the service life, can cause second reagent include concentration be 0.5~1.5g/L ethylenediamine tetrem
Acid disodium and the concentrated sulfuric acid that concentration is 5~10mL/L.The addition of the disodium ethylene diamine tetraacetate and the concentrated sulfuric acid, can be with
The antioxidation of ascorbic acid is improved, so as to improve the stability of the test reagent combination of the total phosphorus in-line analyzer, is prolonged
The service life of the test reagent combination of the total phosphorus in-line analyzer is grown, the shelf-life was up to four months or more.
The present invention also provides a kind of method for measuring total phosphorus content in water sample, this method uses above-mentioned total phosphorus in-line analyzer
Test reagent combination.Wherein, this method comprises the following steps：
The aqueous solution containing 32.5~40g/L potassium peroxydisulfates is configured, so as to which the first reagent be made；Configuration contains 20~25g/
The aqueous solution of L ascorbic acid, so as to prepare the second reagent；Configuration contains 100~115mL/L concentrated sulfuric acids, 22~26g/L molybdic acids
The aqueous solution of salt, 0.3~0.4g/L potassium antimony tartrates, so as to prepare the 3rd reagent；By first reagent, second examination
Agent, the 3rd reagent are respectively placed on the precalculated position of total phosphorus in-line analyzer, and water sample is detected, and are measured total in water sample
Phosphorus content.Wherein described molybdate can be ammonium molybdate or sodium molybdate.
Technical scheme is further elaborated below in conjunction with specific embodiment.
Embodiment 1：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 32.5g/L；Second reagent contains the ascorbic acid that concentration is 20g/L；Institute
It states the 3rd reagent and contains the molybdate that the concentrated sulfuric acid, concentration that concentration is 100mL/L are 22g/L and the winestone that concentration is 0.3g/L
Sour antimony potassium.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：32.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 32.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：20g ascorbic acid is weighed, is dissolved in 1L deionized waters, is made and contains 20g/L ascorbic acid
The second reagent.
The configuration of 3rd reagent：Respectively by the 100mL concentrated sulfuric acids, 22g molybdates, 0.3g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 100mL/L concentrated sulfuric acids, 22g/L molybdates, 0.3g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Embodiment 2：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 37.5g/L；Second reagent contains the ascorbic acid that concentration is 22g/L；Institute
It states the 3rd reagent and contains the molybdate that the concentrated sulfuric acid, concentration that concentration is 110mL/L are 24g/L and the wine that concentration is 0.35g/L
Stone acid antimony potassium.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：37.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 37.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：22g ascorbic acid is weighed, is dissolved in 1L deionized waters, is made and contains 22g/L ascorbic acid
The second reagent.
The configuration of 3rd reagent：Respectively by the 110mL concentrated sulfuric acids, 24g molybdates, 0.35g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 110mL/L concentrated sulfuric acids, 24g/L molybdates, 0.35g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Embodiment 3：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 40g/L；Second reagent contains the ascorbic acid that concentration is 25g/L；It is described
3rd reagent contains the concentrated sulfuric acid that concentration is 115mL/L, the molybdate that concentration is 26g/L and the tartaric acid that concentration is 0.4g/L
Antimony potassium.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：40g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 40g/L potassium peroxydisulfates
The first reagent.
The configuration of second reagent：25g ascorbic acid is weighed, is dissolved in 1L deionized waters, is made and contains 25g/L ascorbic acid
The second reagent.
The configuration of 3rd reagent：Respectively by the 115mL concentrated sulfuric acids, 26g molybdates, 0.4g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 115mL/L concentrated sulfuric acids, 26g/L molybdates, 0.4g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Embodiment 4：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 37.5g/L；Second reagent contains the ascorbic acid, dense that concentration is 22g/L
Spend the disodium ethylene diamine tetraacetate for 0.5g/L, the concentrated sulfuric acid that concentration is 5mL/L；3rd reagent contains concentration for 110mL/
The potassium antimony tartrate that the molybdate and concentration that the concentrated sulfuric acid of L, concentration are 24g/L are 0.35g/L.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：37.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 37.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：Respectively by 22g ascorbic acid, 0.5g disodium ethylene diamine tetraacetates, the 5mL concentrated sulfuric acids, it is dissolved in
In 1L deionized waters, be made containing 22g/L ascorbic acid, 0.5g/L disodium ethylene diamine tetraacetates, 5mL/L the concentrated sulfuric acid second
Reagent.
The configuration of 3rd reagent：Respectively by the 110mL concentrated sulfuric acids, 24g molybdates, 0.35g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 110mL/L concentrated sulfuric acids, 24g/L molybdates, 0.35g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Embodiment 5：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 37.5g/L；Second reagent contains the ascorbic acid, dense that concentration is 22g/L
Spend the disodium ethylene diamine tetraacetate for 1.0g/L, the concentrated sulfuric acid that concentration is 10mL/L；3rd reagent contains concentration and is
The potassium antimony tartrate that the molybdate and concentration that the concentrated sulfuric acid of 110mL/L, concentration are 24g/L are 0.35g/L.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：37.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 37.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：Respectively by 22g ascorbic acid, 1.0g disodium ethylene diamine tetraacetates, the 10mL concentrated sulfuric acids, it is dissolved in
In 1L deionized waters, be made containing 22g/L ascorbic acid, 1.0g/L disodium ethylene diamine tetraacetates, 10mL/L the concentrated sulfuric acid the
Two reagents.
The configuration of 3rd reagent：Respectively by the 110mL concentrated sulfuric acids, 24g molybdates, 0.35g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 110mL/L concentrated sulfuric acids, 24g/L molybdates, 0.35g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Embodiment 6：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 37.5g/L；Second reagent contains the ascorbic acid, dense that concentration is 22g/L
Spend the disodium ethylene diamine tetraacetate for 1.5g/L, the concentrated sulfuric acid that concentration is 10mL/L；3rd reagent contains concentration and is
The potassium antimony tartrate that the molybdate and concentration that the concentrated sulfuric acid of 110mL/L, concentration are 24g/L are 0.35g/L.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：37.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 37.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：Respectively by 22g ascorbic acid, 1.5g disodium ethylene diamine tetraacetates, the 10mL concentrated sulfuric acids, it is dissolved in
In 1L deionized waters, be made containing 22g/L ascorbic acid, 1.5g/L disodium ethylene diamine tetraacetates, 10mL/L the concentrated sulfuric acid the
Two reagents.
The configuration of 3rd reagent：Respectively by the 110mL concentrated sulfuric acids, 24g molybdates, 0.35g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 110mL/L concentrated sulfuric acids, 24g/L molybdates, 0.35g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Comparative example 1：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 30g/L；Second reagent contains the ascorbic acid that concentration is 17g/L；It is described
3rd reagent contains the concentrated sulfuric acid that concentration is 90mL/L, the molybdate that concentration is 20g/L and the tartaric acid that concentration is 0.2g/L
Antimony potassium.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：30g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 30g/L potassium peroxydisulfates
The first reagent.
The configuration of second reagent：17g ascorbic acid is weighed, is dissolved in 1L deionized waters, is made and contains 17g/L ascorbic acid
The second reagent.
The configuration of 3rd reagent：Respectively by the 90mL concentrated sulfuric acids, 20g molybdates, 0.2g potassium antimony tartrates, 1L deionizations are dissolved in
In water, be made containing the 90mL/L concentrated sulfuric acids, 20g/L molybdates, 0.2g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
Comparative example 2：
A kind of test reagent combination of total phosphorus in-line analyzer includes the first reagent, the second reagent and the 3rd reagent, described
First reagent contains the potassium peroxydisulfate that concentration is 42.5g/L；Second reagent contains the ascorbic acid that concentration is 27g/L；Institute
It states the 3rd reagent and contains the molybdate that the concentrated sulfuric acid, concentration that concentration is 120mL/L are 28g/L and the winestone that concentration is 0.5g/L
Sour antimony potassium.
The configuration of the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
The configuration of first reagent：42.5g potassium peroxydisulfates are weighed, are dissolved in 1L deionized waters, is made and contains 42.5g/L over cures
First reagent of sour potassium.
The configuration of second reagent：27g ascorbic acid is weighed, is dissolved in 1L deionized waters, is made and contains 27g/L ascorbic acid
The second reagent.
The configuration of 3rd reagent：Respectively by the 120mL concentrated sulfuric acids, 28g molybdates, 0.5g potassium antimony tartrates, be dissolved in 1L go from
In sub- water, be made containing the 120mL/L concentrated sulfuric acids, 28g/L molybdates, 0.5g/L potassium antimony tartrates the 3rd reagent.
In the present embodiment, the molybdate is ammonium molybdate, in other embodiments, the molybdate or molybdic acid
Sodium.
The method that phosphorus content in water sample is measured using the test reagent combination of the total phosphorus in-line analyzer of the present embodiment is as follows：
In 25 DEG C of room temperature, relative humidity is in 64% indoor environment, by first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
In order to verify each performance of the test reagent combination of total phosphorus in-line analyzer of the present invention, to above three embodiment
And the performance of the test reagent combination in two comparative examples is tested.It is specific as follows：
(1) accuracy is tested
In the environment of 25 DEG C of room temperature, 1 will be implemented to the test reagent combination and comparative example 1 of embodiment 3, comparative example 2
Test reagent combination carries out accuracy test respectively.
Wherein, using Hash Sigma total phosphorus in-line analyzers, respectively to the phosphorus titer (5.0mg/ of four groups of various concentrations
L, 10.0mg/L, 15mg/L, 20mg/L) it is detected, the phosphorus titer of every group of concentration is tested 8 times, is averaged, and is determined with this
The accuracy of the test reagent combination of the present invention (accuracy is represented with relative error).Table 1 is test reagent combination of the invention
The accuracy test result table of phosphorus titer through Hash Sigma total phosphorus in-line analyzer measurement various concentration.
Table 1
As shown in Table 1, the accuracy of test reagent combination of the invention shows the detection reagent group within ± 5%
The accuracy in detection of conjunction is high, has reached the accuracy of laboratory test.
(2) precision is tested
In the environment of 25 DEG C of room temperature, 1 will be implemented to the test reagent combination and comparative example 1 of embodiment 3, comparative example 2
Test reagent combination carries out accuracy test respectively.Wherein, using Hash Sigma total phosphorus in-line analyzers, respectively to four groups not
Phosphorus titer (5.0mg/L, 10.0mg/L, 15mg/L, 20mg/L) with concentration is detected, and the phosphorus titer of every group of concentration is surveyed
Examination 8 times, is averaged, with precision (the precision relative standard deviation table of this test reagent combination for determining the present invention
Show).Table 2 is phosphorus titer of the test reagent combination of the present invention through Hash Sigma total phosphorus in-line analyzer measurement various concentration
Precision test result table.
Table 2
As shown in Table 2, the precision of test reagent combination of the invention shows the detection reagent group within ± 5%
The detection precision of conjunction is high, has reached the precision of laboratory test.
(3) Common Testing of automatic analyzer
In the environment of 25 DEG C of room temperature, Hash Sigma total phosphorus in-line analyzer, HORIBA total phosphorus on-line analyses is respectively adopted
Instrument, just strange WQ-1000 total phosphorus in-line analyzer, Shimadzu TNP-4110 total phosphorus in-line analyzer to embodiment 1 to embodiment 3 and
The test reagent combination of comparative example 1 and comparative example 2 is tested.Table 3 is test reagent combination of the invention through different brands
Total phosphorus in-line analyzer measures the test result table of phosphorus content.Wherein, laboratory is using Germany's 600 spectrophotometrics of Prove measurement
Measure phosphorus content in water sample.
Table 3
As shown in Table 3, the test reagent combination of the embodiment of the present invention 1 to embodiment 3 is using the Kazakhstan of same analysis method
Uncommon Sigma total phosphorus in-line analyzer, HORIBA total phosphorus in-line analyzer, just strange total phosphorus in-line analyzer, Shimadzu total phosphorus divide online
Measurement result is than more consistent in analyzer, and with lab measurements also than more consistent.Therefore, detection reagent group of the invention
Closing has general applicability.
(4) it is applicable in the Common Testing of water quality
In the environment of 25 DEG C of room temperature, it is respectively adopted and implements 1 to the test reagent combination and comparative example 1 of embodiment 3 and right
The test reagent combination of ratio 2 carries out phosphorus content test.Wherein, using Hash Sigma total phosphorus in-line analyzers, respectively to water sample
1st, water sample 2, water sample 3, water sample 4 and water sample 5 are tested.Table 4 exists for the test reagent combination of the present invention through Hash Sigma total phosphorus
Line analysis instrument measures the test result table of the phosphorus content of different water samples.Water sample 1 be paper waste, water sample 2 be wastewater from chemical industry, water sample
3 be pharmacy waste water, and water sample 4 is food wastewater, and water sample 5 is coking wastewater.
Table 4
| Experiment | Water sample 1 | Water sample 2 | Water sample 3 | Water sample 4 | Water sample 5 |
| Laboratory measurements | 3.3 | 1.3 | 4.5 | 1.3 | 4.2 |
| Embodiment 1 | 3.34 | 1.32 | 4.43 | 1.23 | 4.28 |
| Embodiment 2 | 3.32 | 1.36 | 4.53 | 1.35 | 4.21 |
| Embodiment 3 | 3.40 | 1.46 | 4.61 | 1.45 | 4.42 |
| Comparative example 1 | 2.45 | 0.98 | 3.59 | 0.65 | 3.56 |
| Comparative example 2 | 2.46 | 0.92 | 3.64 | 0.72 | 3.49 |
According to table 4, test reagent combination of the invention has the characteristics that versatility to above-mentioned five kinds different water samples,
Being applicable in water quality includes paper waste, wastewater from chemical industry, pharmacy waste water, food wastewater, coking wastewater etc..
(5) stability test
In the environment of 25 DEG C of room temperature, 1 will be implemented respectively to the test reagent combination of embodiment 3 and comparative example 1, comparative example
2 test reagent combination carried out stability test every 30 days, wherein, it is right all using Hash Sigma total phosphorus in-line analyzers
Water sample 1 carries out phosphorus content test.Table 5 measures water for the test reagent combination of the present invention through Hash Sigma total phosphorus in-line analyzer
The stability test result table of the phosphorus content of sample 1.
Table 5
| Experiment | Place 30d | Place 60d | Place 90d | Place 120d | Place 150d |
| Laboratory measurements | 3.3 | 3.3 | 3.3 | 3.3 | 3.3 |
| Embodiment 1 | 3.34 | 3.35 | 3.34 | 1.32 | 1.12 |
| Embodiment 2 | 3.32 | 3.32 | 3.33 | 1.34 | 1.23 |
| Embodiment 3 | 3.40 | 3.42 | 3.41 | 1.42 | 1.31 |
| Embodiment 4 | 3.32 | 3.32 | 3.31 | 3.34 | 1.32 |
| Embodiment 5 | 3.33 | 3.35 | 3.34 | 3.31 | 1.36 |
| Embodiment 6 | 3.31 | 3.32 | 3.35 | 3.34 | 1.38 |
| Comparative example 1 | 2.45 | 2.44 | 1.62 | 0.54 | 0.23 |
| Comparative example 2 | 2.46 | 2.43 | 1.63 | 0.52 | 0.19 |
According to table 5, the shelf-life of test reagent combination prepared by embodiment 1 to embodiment 3 is 3 months, and is implemented
The extended shelf-life for the test reagent combination that example 4 is prepared to embodiment 6 was to 4 months.It is prepared due to embodiment 1 to embodiment 3
Test reagent combination is not added with disodium ethylene diamine tetraacetate and the concentrated sulfuric acid in the second reagent；And prepared by embodiment 4 to embodiment 6
Test reagent combination, add disodium ethylene diamine tetraacetate and the concentrated sulfuric acid in the second reagent, it can be deduced that, in the described second examination
After adding in disodium ethylene diamine tetraacetate and the concentrated sulfuric acid in agent, the shelf-life of test reagent combination of the invention can extend to 4 months.
And generally only 1 month or so the reagent shelf-life of existing total phosphorus In-circiut tester, therefore, test reagent combination of the invention
Stability is preferable.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the scope of the invention, every at this
Under the inventive concept of invention, the equivalent structure transformation made using present specification or directly/be used in other indirectly
Relevant technical field is included in the scope of patent protection of the present invention.
Claims (9)
1. a kind of test reagent combination of total phosphorus in-line analyzer, it is suitable for molybdate spectrophotometry, which is characterized in that institute
Stating test reagent combination includes the first reagent, the second reagent and the 3rd reagent, first reagent contain concentration for 32.5~
The potassium peroxydisulfate of 40g/L；Second reagent contains the ascorbic acid that concentration is 20~25g/L；3rd reagent contains dense
Spend the concentrated sulfuric acid for 100~115mL/L, the molybdate that concentration is 22~26g/L and the tartaric acid that concentration is 0.3~0.4g/L
Antimony potassium.
2. the test reagent combination of total phosphorus in-line analyzer as described in claim 1, which is characterized in that second reagent is also
Contain the disodium ethylene diamine tetraacetate that concentration is 0.5~1.5g/L and the concentrated sulfuric acid that concentration is 5~10mL/L.
3. the test reagent combination of total phosphorus in-line analyzer as claimed in claim 2, which is characterized in that first reagent contains
There is the potassium peroxydisulfate that concentration is 32.5~37.5g/L.
4. the test reagent combination of total phosphorus in-line analyzer as claimed in claim 3, which is characterized in that second reagent contains
There is the ascorbic acid that concentration is 20~22g/L.
5. the test reagent combination of total phosphorus in-line analyzer as claimed in claim 4, which is characterized in that the 3rd reagent contains
There is the concentrated sulfuric acid that concentration is 100~110mL/L.
6. the test reagent combination of total phosphorus in-line analyzer as claimed in claim 5, which is characterized in that the 3rd reagent contains
There is the molybdate that concentration is 22~24g/L.
7. the test reagent combination of total phosphorus in-line analyzer as claimed in claim 6, which is characterized in that the 3rd reagent contains
There is the potassium antimony tartrate that concentration is 0.3~0.35g/L.
8. the test reagent combination of total phosphorus in-line analyzer as described in any one of claim 1 to 7, which is characterized in that described
Molybdate is ammonium molybdate or sodium molybdate.
A kind of 9. method for measuring total phosphorus content in water sample, which is characterized in that this method comprises the following steps：
The aqueous solution containing 32.5~40g/L potassium peroxydisulfates is configured, so as to which the first reagent be made；Configuration resists containing 20~25g/L
The aqueous solution of bad hematic acid, so as to prepare the second reagent；Configuration containing 100~115mL/L concentrated sulfuric acids, 22~26g/L molybdates,
The aqueous solution of 0.3~0.4g/L potassium antimony tartrates, so as to prepare the 3rd reagent；By first reagent, second reagent, institute
It states the 3rd reagent to be respectively placed on the precalculated position of total phosphorus in-line analyzer, water sample is detected, measure total phosphorus in water sample and contain
Amount.
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| CN111239126A (en) * | 2020-03-11 | 2020-06-05 | 深圳市朗诚科技股份有限公司 | Detection reagent combination for phosphate molybdenum antimony resistance method determination and preparation method thereof |
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| CN112362647A (en) * | 2020-11-06 | 2021-02-12 | 洛阳莱博图电子科技有限公司 | Novel prefabricated reagent |
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| CN111239126A (en) * | 2020-03-11 | 2020-06-05 | 深圳市朗诚科技股份有限公司 | Detection reagent combination for phosphate molybdenum antimony resistance method determination and preparation method thereof |
| CN111707661A (en) * | 2020-06-29 | 2020-09-25 | 中国科学院重庆绿色智能技术研究院 | Total phosphorus rapid detection method, required reagent, standard colorimetric card and kit |
| CN112362647A (en) * | 2020-11-06 | 2021-02-12 | 洛阳莱博图电子科技有限公司 | Novel prefabricated reagent |
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