CN107764808A - The method for the middle total phosphorus content measure accuracy that can increase water quality - Google Patents
The method for the middle total phosphorus content measure accuracy that can increase water quality Download PDFInfo
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- CN107764808A CN107764808A CN201610673126.4A CN201610673126A CN107764808A CN 107764808 A CN107764808 A CN 107764808A CN 201610673126 A CN201610673126 A CN 201610673126A CN 107764808 A CN107764808 A CN 107764808A
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Abstract
The invention discloses a kind of method for the middle total phosphorus content measure accuracy that can increase water quality, the sulfuric acid that 25mL density is 1.84g/mL is added in 975mL water；30g sodium hydroxides are dissolved in water and are diluted to 1000mL；Weigh the potassium dihydrogen phosphate that 0.2147 ± 0.001g is let cool in 110 DEG C of dry 2h in drier, it is transferred to after being dissolved with water in 1000mL volumetric flasks, add about 800mL water plus 5mL sulfuric acid is diluted with water to graticule and mixed, this standard liquid of 1.00mL contains 50.0 μ g phosphorus；10.0mL phosphorus standard liquid is transferred in volumetric flask, 1.00mL standard liquids contain 2.0 μ g phosphorus；Add 1 drop phenolphthalein indicator, sodium hydroxide solution is added dropwise to being in just blush, then sulfuric acid solution is added dropwise to make micro- red just decorporate, move in tool plug graded tube, be diluted with water to graticule, determine absorbance, after the absorbance for deducting blank test, the content of phosphorus is checked in from working curve；Calculated by formula.The efficiency high of the assay method, the cycle is short, and measurement result is accurate, meets use of the people subsequently to water body, protects the health of people.
Description
Technical field
The present invention relates to a kind of method, more particularly, to a kind of side for the middle total phosphorus content measure accuracy that can increase water quality
Method.
Background technology
Phosphorus is No. 15 chemical element, symbol P.Period 3 in the periodic table of elements, the VIth race.Phosphorus is present in human body
In all cells, it is the necessary material for maintaining bone and tooth, almost participates in all chemical reactions physiologically.Phosphorus still makes the heart
It is dirty regularly to beat, maintain the normal function of kidney and pass on the important substance of nerve stimulation.When there is no phosphorus, nicotinic acid（Also known as
Vitamin B3）It can not be absorbed；The normal function of phosphorus needs vitamin（Vitamin food）D and calcium（Calcium food）To maintain.
Phosphorus is found to be present in the universe residue after fixed star explodes first.Newest observation to relic of supernova thing Cassiopeia A is taken off
Newest evidence existing for phosphorus is shown.It is one of two big elements found in deep space, or may provide relevant life to scientist
The clue of possibility in universe.There is very abundant phosphorus in food, therefore it is rare, phosphorus intake or the deficiency absorbed that phosphorus, which lacks,
Hypophosphatemia can occur, cause red blood cell, leucocyte, hematoblastic exception, osteomalacia；Because of disease or excessive intake phosphorus,
Hyperphosphatemia will be caused, blood calcium reduction in blood is caused osteoporosis.Phosphate fertilizer can promote tomato bud differentiation, bloom ahead of time
As a result, promote seedlings root growth and improve fruit quality.When lacking phosphorus, young shoot and root growth are slow, and plant is short and small, and leaf color is dark
It is green, matt, back side purple.Due to the use of phosphate fertilizer so that phosphorus content greatly increases in water body, and this will cause water quality eutrophy
Change, influence water quality, human body, which is drunk or contacted, causes body to injure, it is therefore desirable to which the phosphorus content in water quality is surveyed
It is fixed, and existing assay method efficiency is low, cycle length, and also the resultant error determined is very big.
The content of the invention
It is an object of the invention to overcome the above-mentioned existing assay method efficiency to phosphorus content in water quality low, cycle length, and
And measure resultant error it is very big the problem of, devise a kind of method for the middle total phosphorus content measure accuracy that can increase water quality,
The efficiency high of the assay method, the cycle is short, and measurement result is accurate, meets use of the people subsequently to water body, protects people
Health, it is low to solve the existing assay method efficiency to phosphorus content in water quality, cycle length, and the resultant error determined
The problem of very big.
The purpose of the present invention is achieved through the following technical solutions：The side for the middle total phosphorus content measure accuracy that can increase water quality
Method, comprise the following steps：
（1）Preparation of reagents：The sulfuric acid that 25mL density is 1.84g/mL is added in 975mL water；30g sodium hydroxides are dissolved in water
And it is diluted to 1000mL；250g sodium hydroxides are dissolved in water and are diluted to 1000mL；8g potassium peroxydisulfates are dissolved in water, and diluted
To 100mL；8g ascorbic acid is dissolved in water, and is diluted to 100mL, and this solution is stored in the reagent bottle of brown, can at cold place
Stablize several weeks；11g ammonium molybdates are dissolved in 100mL water；0.32g potassium antimony tartrates are dissolved in 100mL water, in the case where being stirred continuously
Ammonium molybdate solution is added in 300mL sulfuric acid slowly, adds antimony tartrate potassium solution and is well mixed, this solution is stored in brown
In reagent bottle, it can be preserved two months at cold place；Weigh the phosphorus that 0.2147 ± 0.001g is let cool in 110 DEG C of dry 2h in drier
Acid dihydride potassium, it is transferred to after being dissolved with water in 1000mL volumetric flasks, adds about 800mL water plus 5mL sulfuric acid is diluted with water to mark
Line simultaneously mixes, and this standard liquid of 1.00mL contains 50.0 μ g phosphorus；10.0mL phosphorus standard liquid is transferred in 250mL volumetric flasks,
It is diluted with water to graticule and mixes, this standard liquid of 1.00mL contains 2.0 μ g phosphorus；0.5g phenolphthalein is dissolved in 50mL95% ethanol；
（2）Sample preparation：The pH value that 1mL sulfuric acid adjusts sample is added after taking 500mL water samples, is allowed to be less than or equal to 1, or not
Add any reagent to be preserved in cold place, take 25mL samples in tool fill in graded tube in, should carefully be shaken up when taking, with obtain dissolving part and
Floating parts are respectively provided with representational sample；
（3）Determination step：Alkaline potassium per-sulfate digestion：Add 4mL potassium peroxydisulfates into sample, after the lid for having plug graded tube is stoppered, use
One napkin and line tighten glass stopper, are placed on to be placed in high pressure steam boiler in large beaker and heat, and treat that pressure reaches 1.1kg/
cm2, when relevant temperature is 120 DEG C, stopping heating after 30min is kept, after pressure gauge reading is down to zero, taking-up is let cool, then
It is diluted with water to graticule；25mL samples are taken in conical flask, addend grain bead, add 2mL nitric acid to heat concentration on electric hot plate
To 10mL, after cold plus 5mL nitric acid, reheating are concentrated into 10mL, let cool, add 3mL perchloric acid, be heated to perchloric acid and emit white cigarette, this
When can on conical flask plus small funnel or regulation electric plate temperature, digestion solution is maintained the reflux for state in conical flask inwall, until
Remaining 3~4mL, lets cool, adds water 10mL, adds 1 drop phenolphthalein indicator, and sodium hydroxide solution is added dropwise to being in just blush, then be added dropwise
Sulfuric acid solution make it is micro- it is red just decorporate, fully mix, move to tool plug graded tube in, be diluted with water to graticule, disappear respectively to each part
Solving and the mixing of 1mL ascorbic acid solutions is added in liquid, after 30s plus 2mL molybdate solutions fully mix, after placing 15min at room temperature,
The use of light path is 30mm cuvettes, under 700nm wavelength, reference is done with water, determines absorbance, deducts the absorbance of blank test
Afterwards, the content of phosphorus is checked in from working curve, takes 7 brace plug graded tubes to be separately added into 0.0,0.50,1.00,3.00,5.00,
10.0,15.0mL phosphate standard solution, add water to 25mL, are then handled by determination step, do reference with water, measure is inhaled
Luminosity, after the absorbance for deducting blank test, and the content drawing curve of corresponding phosphorus；
（4）As a result represent：Total phosphorus content is represented with C (mg/L), is calculated as follows：
C=m/V
In formula：M --- sample measures phosphorus content, μ g；
V --- measurement sample volume, mL.
In summary, the beneficial effects of the invention are as follows：The efficiency high of the assay method, the cycle is short, and measurement result is accurate
Really, meet use of the people subsequently to water body, protect the health of people, solve the existing measure to phosphorus content in water quality
The problem of method efficiency is low, cycle length, and the resultant error determined is very big.
Embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited only to
This.
Embodiment：
The method for the middle total phosphorus content measure accuracy that can increase water quality, comprises the following steps：
（1）Preparation of reagents：The sulfuric acid that 25mL density is 1.84g/mL is added in 975mL water；30g sodium hydroxides are dissolved in water
And it is diluted to 1000mL；250g sodium hydroxides are dissolved in water and are diluted to 1000mL；8g potassium peroxydisulfates are dissolved in water, and diluted
To 100mL；8g ascorbic acid is dissolved in water, and is diluted to 100mL, and this solution is stored in the reagent bottle of brown, can at cold place
Stablize several weeks；11g ammonium molybdates are dissolved in 100mL water；0.32g potassium antimony tartrates are dissolved in 100mL water, in the case where being stirred continuously
Ammonium molybdate solution is added in 300mL sulfuric acid slowly, adds antimony tartrate potassium solution and is well mixed, this solution is stored in brown
In reagent bottle, it can be preserved two months at cold place；Weigh the phosphorus that 0.2147 ± 0.001g is let cool in 110 DEG C of dry 2h in drier
Acid dihydride potassium, it is transferred to after being dissolved with water in 1000mL volumetric flasks, adds about 800mL water plus 5mL sulfuric acid is diluted with water to mark
Line simultaneously mixes, and this standard liquid of 1.00mL contains 50.0 μ g phosphorus；10.0mL phosphorus standard liquid is transferred in 250mL volumetric flasks,
It is diluted with water to graticule and mixes, this standard liquid of 1.00mL contains 2.0 μ g phosphorus；0.5g phenolphthalein is dissolved in 50mL95% ethanol；
（2）Sample preparation：The pH value that 1mL sulfuric acid adjusts sample is added after taking 500mL water samples, is allowed to be less than or equal to 1, or not
Add any reagent to be preserved in cold place, take 25mL samples in tool fill in graded tube in, should carefully be shaken up when taking, with obtain dissolving part and
Floating parts are respectively provided with representational sample；
（3）Determination step：Alkaline potassium per-sulfate digestion：Add 4mL potassium peroxydisulfates into sample, after the lid for having plug graded tube is stoppered, use
One napkin and line tighten glass stopper, are placed on to be placed in high pressure steam boiler in large beaker and heat, and treat that pressure reaches 1.1kg/
cm2, when relevant temperature is 120 DEG C, stopping heating after 30min is kept, after pressure gauge reading is down to zero, taking-up is let cool, then
It is diluted with water to graticule；25mL samples are taken in conical flask, addend grain bead, add 2mL nitric acid to heat concentration on electric hot plate
To 10mL, after cold plus 5mL nitric acid, reheating are concentrated into 10mL, let cool, add 3mL perchloric acid, be heated to perchloric acid and emit white cigarette, this
When can on conical flask plus small funnel or regulation electric plate temperature, digestion solution is maintained the reflux for state in conical flask inwall, until
Remaining 3~4mL, lets cool, adds water 10mL, adds 1 drop phenolphthalein indicator, and sodium hydroxide solution is added dropwise to being in just blush, then be added dropwise
Sulfuric acid solution make it is micro- it is red just decorporate, fully mix, move to tool plug graded tube in, be diluted with water to graticule, disappear respectively to each part
Solving and the mixing of 1mL ascorbic acid solutions is added in liquid, after 30s plus 2mL molybdate solutions fully mix, after placing 15min at room temperature,
The use of light path is 30mm cuvettes, under 700nm wavelength, reference is done with water, determines absorbance, deducts the absorbance of blank test
Afterwards, the content of phosphorus is checked in from working curve, takes 7 brace plug graded tubes to be separately added into 0.0,0.50,1.00,3.00,5.00,
10.0,15.0mL phosphate standard solution, add water to 25mL, are then handled by determination step, do reference with water, measure is inhaled
Luminosity, after the absorbance for deducting blank test, and the content drawing curve of corresponding phosphorus；
（4）As a result represent：Total phosphorus content is represented with C (mg/L), is calculated as follows：
C=m/V
In formula：M --- sample measures phosphorus content, μ g；
V --- measurement sample volume, mL.
The efficiency high of the assay method, the cycle is short, and measurement result is accurate, meets use of the people subsequently to water body,
The health of people is protected, it is low to solve the existing assay method efficiency to phosphorus content in water quality, cycle length, and determine
The problem of resultant error is very big.
It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to
Any simply modification, the equivalent variations substantially made according to the technology of the present invention, method to above example, each fall within the present invention
Protection domain within.
Claims (1)
1. the method for the middle total phosphorus content measure accuracy that can increase water quality, it is characterised in that comprise the following steps：
（1）Preparation of reagents：The sulfuric acid that 25mL density is 1.84g/mL is added in 975mL water；30g sodium hydroxides are dissolved in water
And it is diluted to 1000mL；250g sodium hydroxides are dissolved in water and are diluted to 1000mL；8g potassium peroxydisulfates are dissolved in water, and diluted
To 100mL；8g ascorbic acid is dissolved in water, and is diluted to 100mL, and this solution is stored in the reagent bottle of brown, can at cold place
Stablize several weeks；11g ammonium molybdates are dissolved in 100mL water；0.32g potassium antimony tartrates are dissolved in 100mL water, in the case where being stirred continuously
Ammonium molybdate solution is added in 300mL sulfuric acid slowly, adds antimony tartrate potassium solution and is well mixed, this solution is stored in brown
In reagent bottle, it can be preserved two months at cold place；Weigh the phosphorus that 0.2147 ± 0.001g is let cool in 110 DEG C of dry 2h in drier
Acid dihydride potassium, it is transferred to after being dissolved with water in 1000mL volumetric flasks, adds about 800mL water plus 5mL sulfuric acid is diluted with water to mark
Line simultaneously mixes, and this standard liquid of 1.00mL contains 50.0 μ g phosphorus；10.0mL phosphorus standard liquid is transferred in 250mL volumetric flasks,
It is diluted with water to graticule and mixes, this standard liquid of 1.00mL contains 2.0 μ g phosphorus；0.5g phenolphthalein is dissolved in 50mL95% ethanol；
（2）Sample preparation：The pH value that 1mL sulfuric acid adjusts sample is added after taking 500mL water samples, is allowed to be less than or equal to 1, or not
Add any reagent to be preserved in cold place, take 25mL samples in tool fill in graded tube in, should carefully be shaken up when taking, with obtain dissolving part and
Floating parts are respectively provided with representational sample；
（3）Determination step：Alkaline potassium per-sulfate digestion：Add 4mL potassium peroxydisulfates into sample, after the lid for having plug graded tube is stoppered, use
One napkin and line tighten glass stopper, are placed on to be placed in high pressure steam boiler in large beaker and heat, and treat that pressure reaches 1.1kg/
cm2, when relevant temperature is 120 DEG C, stopping heating after 30min is kept, after pressure gauge reading is down to zero, taking-up is let cool, then
It is diluted with water to graticule；25mL samples are taken in conical flask, addend grain bead, add 2mL nitric acid to heat concentration on electric hot plate
To 10mL, after cold plus 5mL nitric acid, reheating are concentrated into 10mL, let cool, add 3mL perchloric acid, be heated to perchloric acid and emit white cigarette, this
When can on conical flask plus small funnel or regulation electric plate temperature, digestion solution is maintained the reflux for state in conical flask inwall, until
Remaining 3~4mL, lets cool, adds water 10mL, adds 1 drop phenolphthalein indicator, and sodium hydroxide solution is added dropwise to being in just blush, then be added dropwise
Sulfuric acid solution make it is micro- it is red just decorporate, fully mix, move to tool plug graded tube in, be diluted with water to graticule, disappear respectively to each part
Solving and the mixing of 1mL ascorbic acid solutions is added in liquid, after 30s plus 2mL molybdate solutions fully mix, after placing 15min at room temperature,
The use of light path is 30mm cuvettes, under 700nm wavelength, reference is done with water, determines absorbance, deducts the absorbance of blank test
Afterwards, the content of phosphorus is checked in from working curve, takes 7 brace plug graded tubes to be separately added into 0.0,0.50,1.00,3.00,5.00,
10.0,15.0mL phosphate standard solution, add water to 25mL, are then handled by determination step, do reference with water, measure is inhaled
Luminosity, after the absorbance for deducting blank test, and the content drawing curve of corresponding phosphorus；
（4）As a result represent：Total phosphorus content is represented with C (mg/L), is calculated as follows：
C=m/V
In formula：M --- sample measures phosphorus content, μ g；
V --- measurement sample volume, mL.
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| CN201610673126.4A CN107764808A (en) | 2016-08-16 | 2016-08-16 | The method for the middle total phosphorus content measure accuracy that can increase water quality |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956582A (en) * | 2018-05-16 | 2018-12-07 | 江苏盐城环保科技城重金属防治研究中心 | A kind of emission spectrometry method of high-copper Phosphorus From Wastewater content |
| CN108982404A (en) * | 2018-08-23 | 2018-12-11 | 睿藻生物科技（苏州）有限公司 | It is a kind of for measuring the reagent and measurement method of total Phos in aqueous liquid sample |
| 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 |
| CN112540076A (en) * | 2020-11-04 | 2021-03-23 | 飞鸣科学仪器（武汉）有限公司 | Detection reagent for detecting total phosphorus content in wastewater and preparation process thereof |
-
2016
- 2016-08-16 CN CN201610673126.4A patent/CN107764808A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956582A (en) * | 2018-05-16 | 2018-12-07 | 江苏盐城环保科技城重金属防治研究中心 | A kind of emission spectrometry method of high-copper Phosphorus From Wastewater content |
| CN108982404A (en) * | 2018-08-23 | 2018-12-11 | 睿藻生物科技（苏州）有限公司 | It is a kind of for measuring the reagent and measurement method of total Phos in aqueous liquid sample |
| 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 |
| CN112540076A (en) * | 2020-11-04 | 2021-03-23 | 飞鸣科学仪器（武汉）有限公司 | Detection reagent for detecting total phosphorus content in wastewater and preparation process thereof |
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Application publication date: 20180306 |