CN108982404A - It is a kind of for measuring the reagent and measurement method of total Phos in aqueous liquid sample - Google Patents
It is a kind of for measuring the reagent and measurement method of total Phos in aqueous liquid sample Download PDFInfo
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- CN108982404A CN108982404A CN201810965343.XA CN201810965343A CN108982404A CN 108982404 A CN108982404 A CN 108982404A CN 201810965343 A CN201810965343 A CN 201810965343A CN 108982404 A CN108982404 A CN 108982404A
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- reagent
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- aqueous liquid
- liquid sample
- solid
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 84
- 239000007788 liquid Substances 0.000 title claims abstract description 49
- 238000000691 measurement method Methods 0.000 title claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007787 solid Substances 0.000 claims abstract description 25
- 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 24
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 17
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 17
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 17
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229930003268 Vitamin C Natural products 0.000 claims abstract description 12
- 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 12
- 235000019154 vitamin C Nutrition 0.000 claims abstract description 12
- 239000011718 vitamin C Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 18
- 238000002835 absorbance Methods 0.000 claims description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims description 13
- 239000011574 phosphorus Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 238000005259 measurement Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000001473 noxious effect Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000036632 reaction speed Effects 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- JKMHFZQWWAIEOD-UHFFFAOYSA-N 2-[4-(2-hydroxyethyl)piperazin-1-yl]ethanesulfonic acid Chemical compound OCC[NH+]1CCN(CCS([O-])(=O)=O)CC1 JKMHFZQWWAIEOD-UHFFFAOYSA-N 0.000 description 1
- RJNYNDHYSJRRDW-UHFFFAOYSA-N 4-(pyridin-2-yldiazenyl)benzene-1,3-diol Chemical compound OC1=CC(O)=CC=C1N=NC1=CC=CC=N1 RJNYNDHYSJRRDW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000007995 HEPES buffer Substances 0.000 description 1
- -1 Pb2+ ion Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- 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
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of for measuring the reagent and measurement method of total Phos in aqueous liquid sample, which includes liquid reagent and solid reagent, and liquid reagent includes the following parts by weight: 30-35 parts of sulfuric acid, 5-7 parts of ammonium molybdate and 1000 parts of water;Solid reagent includes the following parts by weight: 34-40 parts and 1 part of potassium antimony tartrate of vitamin C.The advantages that reagent prepared by the present invention, which has, prepares simplicity, and reaction speed is fast, and storage time length, stability are strong after preparation, easy to use, and as a result accurately, anti-chemistry, optical interference ability are stronger, is free of noxious material.
Description
Technical field
The invention belongs to the field of measuring technique of Phos, and in particular to one kind is total inorganic in aqueous liquid sample for measuring
The reagent and measurement method of phosphorus, are widely used in farming and animal husbandry, feed flow and scientific research field.
Background technique
The detection of Phos is in agricultural, industry, makes in the fields such as scientific research essential.The survey of many water body total phosphorus contents
It is fixed, and by being converted to Phos by organic phosphorus and further being measured.
Currently, about measurement Phos method it is more, such as filed on January 9th, 2009, notification number be
The Chinese invention patent of CN101477059B provides a kind of method of directly measurement inorganic phosphorus in water solution, is based on divalent lead
Pb2+ ion is that color developing agent is direct in the HEPES buffer solution that pH is 7.0 with 4- (2_ pyridylazo) resorcinol (PAR)
Phos is detected to qualitative, quantitative, but solution is prepared and operating process is complicated, and needs in reagent using to human body and ring
There is the lead of high risks in border.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of preparations simply, reaction speed is fast, storage time is long,
And the reagent and measurement method for being used to measure total Phos in aqueous liquid sample without noxious material.
In order to achieve the above object, technical scheme is as follows:
The present invention provides a kind of for measuring the reagent of total Phos in aqueous liquid sample, including liquid reagent and solid examination
Agent, liquid reagent include the following parts by weight:
Sulfuric acid: 30-35 parts
Ammonium molybdate: 5-7 parts
Water: 1000 parts
Solid reagent includes the following parts by weight:
Vitamin C: 34-40 parts
Potassium antimony tartrate: 1 part.
As a preferred option, reagent when in use, first mixing liquid reagent and solid reagent, after mixing, then plus
Enter aqueous liquid sample.
As a preferred option, after liquid reagent and solid reagent mixing in reagent each ingredient concentration are as follows: sulfuric acid
17.86mL/L, ammonium molybdate 6g/L, potassium antimony tartrate 0.143g/L, vitamin C 5.28g/L.
As a preferred option, the present invention also provides a kind of measurement methods of Phos total in aqueous liquid sample, including with
Lower step:
The configuration of reagent: being configured to sulfuric acid solution for sulfuric acid addition water, ammonium molybdate is dissolved in water is configured to ammonium molybdate solution,
Then sulfuric acid solution is mixed with ammonium molybdate solution by the deal described in claim 1, adds water to be configured to liquid reagent, refills
It is stand-by to enter a container that is clean, not reacting with reagent;
Weigh potassium antimony tartrate and vitamin C, be mixed and made into solid reagent, be then charged into one it is clean, not with reagent
The container of reaction is stand-by;
The use of reagent: in use, be first uniformly mixed the liquid reagent configured according to the above method and solid reagent, then plus
Enter aqueous liquid sample to be measured, is uniformly mixed;
It waits 20-30 minutes, is then to wavelength using the mixture of absorption spectrophotometry measurement reagent and aqueous liquid sample
The absorbance of the infrared light of 882nm;By measuring resulting absorbance, the inorganic standard phosphorus solution containing known concentration and examination are compared
To the absorbance for the infrared light that wavelength is 882nm after agent reaction, the concentration of total Phos in sample, calculation method are calculated
Are as follows: suction of total inorganic phosphorus concentration=standard solution inorganic phosphorus concentration ÷ standard solution to the infrared light that wavelength is 882nm in sample
Luminosity × reagent and the mixture of aqueous liquid sample are the absorbance of the infrared light of 882nm to wavelength.
The invention has the following advantages: reagent prepared by the present invention, which has, prepares simplicity, reaction speed is fast, after preparation
Storage time is long, stability is strong, easy to use, and as a result accurately, anti-chemistry, optical interference ability are stronger, without noxious material etc.
Advantage.
Detailed description of the invention
Fig. 1 is the measurement result using the measurement method measurement Phos standard solution of total Phos disclosed by the invention.
Specific embodiment
The preferred embodiment that the invention will now be described in detail with reference to the accompanying drawings.
Embodiment 1
In order to reach the purpose of the present invention, provided in one of embodiment of the invention a kind of water-soluble for measuring
The reagent of total Phos in liquid sample, including liquid reagent and solid reagent, liquid reagent include the following parts by weight:
Sulfuric acid: 30 parts
Ammonium molybdate: 5 parts
Water: 1000 parts
Solid reagent includes the following parts by weight:
Vitamin C: 34 parts
Potassium antimony tartrate: 1 part.
Embodiment 2
In order to reach the purpose of the present invention, provided in one of embodiment of the invention a kind of water-soluble for measuring
The reagent of total Phos in liquid sample, including liquid reagent and solid reagent, liquid reagent include the following parts by weight:
Sulfuric acid: 32 parts
Ammonium molybdate: 6 parts
Water: 1000 parts
Solid reagent includes the following parts by weight:
Vitamin C: 40 parts
Potassium antimony tartrate: 1 part.
Embodiment 3
In order to reach the purpose of the present invention, provided in one of embodiment of the invention a kind of water-soluble for measuring
The reagent of total Phos in liquid sample, including liquid reagent and solid reagent, liquid reagent include the following parts by weight:
Sulfuric acid: 35 parts
Ammonium molybdate: 7 parts
Water: 1000 parts
Solid reagent includes the following parts by weight:
Vitamin C: 40 parts
Potassium antimony tartrate: 1 part.
Wherein, when in use, first mixing liquid reagent and solid reagent add aqueous solution sample after mixing to reagent
This.
In addition, after body reagent and solid reagent mixing in reagent each ingredient concentration are as follows: sulfuric acid 17.86mL/L, molybdic acid
Ammonium 6g/L, potassium antimony tartrate 0.143g/L, vitamin C 5.28g/L.
In order to further optimize implementation result of the invention, in another embodiment of the invention, the present invention is also
A kind of measurement method of total Phos in aqueous liquid sample is provided, comprising the following steps:
The configuration of reagent: it is 250mL that the 35mL concentrated sulfuric acid (98%) addition water, which is configured to total amount, and concentration is the sulfuric acid of 2.5M
Solution.4g ammonium molybdate is dissolved in water, is configured to the ammonium molybdate solution that total amount is 100mL.By the above-mentioned sulfuric acid solution of 250mL and 75mL
Above-mentioned ammonium molybdate solution mixing, adds water to be configured to the liquid reagent that total amount is 500mL.2mL is taken to be packed into PP plastic containers stand-by.Claim
The potassium antimony tartrate for taking 0.572mg weighs 0.021g vitamin C, and two kinds of solid matters are mixed and made into solid reagent, are packed into PP
Container is stand-by.
The use of reagent: in use, being first uniformly mixed the 2mL liquid reagent and solid reagent that configure according to the above method.
10mL aqueous liquid sample to be measured is added, is uniformly mixed.It waits 30 minutes, then using absorption spectrophotometry measurement reagent and sample
Mixture to wavelength be 882nm infrared light absorbance.By measuring resulting absorbance, compare containing known concentration
Inorganic standard phosphorus solution reacted with reagent after to wavelength be 882nm infrared light absorbance (as shown in Figure 1), calculate sample
In total Phos concentration.Its calculation method are as follows: total inorganic phosphorus concentration=standard solution inorganic phosphorus concentration ÷ standard is molten in sample
Liquid is the infrared of 882nm to wavelength to the absorbance × reagent for the infrared light that wavelength is 882nm and the mixture of aqueous liquid sample
The absorbance of light.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, these belong to the present invention
Protection scope.
Claims (4)
1. a kind of for measuring the reagent of total Phos in aqueous liquid sample, which is characterized in that tried including liquid reagent and solid
Agent, liquid reagent include the following parts by weight:
Sulfuric acid: 30-35 parts
Ammonium molybdate: 5-7 parts
Water: 1000 parts
Solid reagent includes the following parts by weight:
Vitamin C: 34-40 parts
Potassium antimony tartrate: 1 part.
2. according to claim 1 for measuring the reagent of total Phos in aqueous liquid sample, which is characterized in that reagent exists
In use, first mixing liquid reagent and solid reagent add aqueous liquid sample after mixing.
3. according to claim 1 for measuring the reagent of total Phos in aqueous liquid sample, which is characterized in that liquid examination
After agent and solid reagent mixing in reagent each ingredient concentration are as follows: sulfuric acid 17.86mL/L, ammonium molybdate 6g/L, potassium antimony tartrate
0.143g/L, vitamin C 5.28g/L.
4. the measurement method of total Phos in a kind of aqueous liquid sample, which comprises the following steps:
The configuration of reagent: sulfuric acid addition water is configured to sulfuric acid solution, ammonium molybdate is dissolved in water is configured to ammonium molybdate solution, then
Sulfuric acid solution is mixed with ammonium molybdate solution by the deal described in claim 1, adds water to be configured to liquid reagent, is reloaded into dry
Container that is net, not reacting with reagent is stand-by;
Weigh potassium antimony tartrate and vitamin C, be mixed and made into solid reagent, be then charged into one it is clean, do not react with reagent
Container it is stand-by;
The use of reagent: in use, first the liquid reagent configured according to the above method and solid reagent are uniformly mixed, add to
Aqueous liquid sample is surveyed, is uniformly mixed;
It waits 20-30 minutes, the use of absorption spectrophotometry measurement reagent and the mixture of aqueous liquid sample is then 882nm to wavelength
Infrared light absorbance;By measuring resulting absorbance, inorganic standard phosphorus solution and reagent of the comparison containing known concentration are anti-
Should after to wavelength be 882nm infrared light absorbance, calculate the concentration of total Phos in sample, calculation method are as follows: sample
In this total inorganic phosphorus concentration=standard solution inorganic phosphorus concentration ÷ standard solution to the absorbance of the infrared light that wavelength is 882nm ×
Reagent and the mixture of aqueous liquid sample are the absorbance of the infrared light of 882nm to wavelength.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105424628A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Determination method for total phosphorus in water |
CN107764808A (en) * | 2016-08-16 | 2018-03-06 | 陈飞 | The method for the middle total phosphorus content measure accuracy that can increase water quality |
CN107782722A (en) * | 2016-08-26 | 2018-03-09 | 刘荣伟 | Method based on middle total phosphorus content determination efficiency of increasing water quality |
CN108107012A (en) * | 2018-02-24 | 2018-06-01 | 深圳市长协新能源科技有限公司 | A kind of test reagent combination of total phosphorus in-line analyzer and its method for measuring total phosphorus content in water sample |
-
2018
- 2018-08-23 CN CN201810965343.XA patent/CN108982404A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105424628A (en) * | 2015-12-10 | 2016-03-23 | 苏州国环环境检测有限公司 | Determination method for total phosphorus in water |
CN107764808A (en) * | 2016-08-16 | 2018-03-06 | 陈飞 | The method for the middle total phosphorus content measure accuracy that can increase water quality |
CN107782722A (en) * | 2016-08-26 | 2018-03-09 | 刘荣伟 | Method based on middle total phosphorus content determination efficiency of increasing water quality |
CN108107012A (en) * | 2018-02-24 | 2018-06-01 | 深圳市长协新能源科技有限公司 | A kind of test reagent combination of total phosphorus in-line analyzer and its method for measuring total phosphorus content in water sample |
Non-Patent Citations (1)
Title |
---|
雷衍之等: "《养殖水环境化学实验》", 31 July 2006, 中国农业出版社 * |
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Application publication date: 20181211 |