CN104502295B - On-line monitoring method for total phosphorus in water - Google Patents
On-line monitoring method for total phosphorus in water Download PDFInfo
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- CN104502295B CN104502295B CN201510012716.8A CN201510012716A CN104502295B CN 104502295 B CN104502295 B CN 104502295B CN 201510012716 A CN201510012716 A CN 201510012716A CN 104502295 B CN104502295 B CN 104502295B
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Abstract
The invention provides an on-line monitoring method for total phosphorus in water, and aims at monitoring a pollution accident on a scene. The on-line monitoring method comprises the following steps: sampling; determining an acid-alkali ratio; shaking up; carrying out alkaline digestion; cooling; carrying out acidic digestion; cooling; adding an ammonium molybdate solution into a first digestion container and a second digestion container, and sufficiently mixing; measuring the contents X and Y of the total phosphorus of the first digestion container and the second digestion container by adopting an spectrophotometric method; and calculating the total phosphorus. According to the on-line monitoring method, the total phosphorus value of a polluted scene water body is rapidly obtained under the condition that complicated analysis including chromatographic analysis and the like is not carried out. The potential of hydrogen of a water body to be detected is considered, and the potential of the hydrogen is determined in a measurement process and a result is compensated, so that the measured result is relatively close to the result obtained by adopting an ion chromatography.
Description
Technical field
The present invention relates to a kind of water quality detection method, more particularly, to a kind of water quality total phosphorus on-line monitoring method.
Background technology
Phosphorus in environment water is mainly with element phosphor, organophosphors (phosphate for combining with organic group), orthophosphate, contracting
Close sulfate, pyrophosphate, the form such as metaphosphate to exist, its main source is sanitary sewage, chemical fertilizer, organophosphorus pesticide and near
For phosphate buider used by detergent etc..Total phosphorus is in unit volume (typically in terms of mL) water sample in all phosphorus-containing compounds
Phosphorus content, total phosphorus is the important water quality monitoring parameter for controlling body eutrophication, is drinking, go sight-seeing and cultivating for water conservation
Deng Development volue must effective monitoring one of water quality parameter, be that monitoring water environment must survey one of project.
At present, total phosphorus monitoring instrument adopts national standards laboratory analysis method, i.e. ammonium molybdate spectrophotometric method mostly, its
Principle is to clear up water sample with potassium peroxydisulfate (or nitric acid-perchloric acid), is combined by pyrophosphate, metaphosphate and with Organic substance
The phosphorus that the various forms such as phosphate are present all is oxidized to inorganic orthophosphate.Orthophosphate generates phosphorus molybda with ammonium molybdate reaction
Polyacid, adds ascorbic acid to be reduced it, generates blue complex, and total phosphorus content is detected at 700nm with spectrophotography.
The method sample needs to clear up reaction in high temperature, high-pressure bottle, and detection process is complicated, takes excessive.
Additionally, with regard to current total phosphorus detection additive method for, such as Zinc chloride cell, the chromatography of ions,
Gas ions spectrum-spectrometer analysis etc., these methods or operating procedure redundant and complicated, or interference factor is more, its intermediate ion color
The detection methods such as spectrometry, plasma spectrometry-spectrometer analysis are needed using instrument costly, and are had to operator
Very high professional skill is required, and mostly adopts large-sized analytic instrument, can only be completed in laboratory, it is impossible to meet contamination accident
Field monitoring.
The content of the invention
In order to overcome above-mentioned deficiency of the prior art, the invention provides a kind of water quality total phosphorus on-line monitoring method, bag
Include following steps：
(1) sample：200ml water bodys to be measured are gathered by disposable tank；
(2) acid/base ratio is determined：Take 100ml water bodys to be measured and determine acid-base value, so as to be calculated the pH of water body to be measured
Value；
(3) process is shaken up：Disposable tank is at the uniform velocity shaken, and 2ml sodium perchlorate is at the uniform velocity instilled while shake
Solution, treats that instillation is finished, and respectively takes 30ml respectively in two sealable digestion containers, wherein the first digestion container alkali resistance,
Second digestion container acid resistance；
(4) alkalescence is cleared up：Alkaline gas are passed through in the first digestion container, and make the temperature of the first digestion container at 6 points
First degree Celsius is uniformly increased in clock, then, on first degree Celsius 10 minutes is incubated；
(5) cool down：In 5 minutes, the first digestion container after clearing up cools to 25 degrees Celsius, and in the process to
Noble gases are passed through in first digestion container；
(6) acidity is cleared up：Sour gas is passed through in the second digestion container, and makes the temperature of the second digestion container at 4 points
Second degree Celsius is uniformly increased in clock, then, on second degree Celsius 12 minutes is incubated；
(7) cool down：In 5 minutes, the second digestion container after clearing up cools to 25 degrees Celsius, and in the process to
Noble gases are passed through in second digestion container；
(8) in the first digestion container and the second digestion container ammonium molybdate solution is separately added into respectively, is sufficiently mixed；
(9) using the digestion container of metric measurement first and the respective total phosphorus content X and Y of the second digestion container；
(10) when the pH value of water body to be measured is more than 7, total phosphorus content=(| | the pH value of water body to be measured | | the * X of water body to be measured
+ (| | the pH value of water body to be measured | |+1) * Y)/(2* | | the pH value of water body to be measured | |)；When the pH value of water body to be measured is less than 7, treat
Total phosphorus content=((| | the pH value of water body to be measured | | -1) * X+ (| | the pH value of water body to be measured | |+1) the * Y) of survey water body/(2* | | treat
Survey the pH value of water body | |).
Further, in the step (2), using the acid solution or sodium hydroxide solution of chlorate anions acid/base ratio drop is carried out
It is fixed.
Further, described first degree Celsius is 120 degrees Celsius~200 degrees Celsius.
Further, described second degree Celsius is 80 degrees Celsius~150 degrees Celsius.
Further, the noble gases are neon.
Further, also included before step (8)：With distilled water by the first digestion container and the second digestion container
Solution is settled to respectively 10ml.
Further, the content of the ammonium molybdate solution is 3ml.
Further, before ammonium molybdate solution is added, it is additionally added ascorbic acid solution.
The invention has the beneficial effects as follows：Dirt can be quickly obtained in the case where the complicated analysis such as chromatography is not carried out
The total phosphorus value of the live water body of dye.And, the present invention take into account the acid-base value of water body to be measured, and to acid-base value in measurement process
It is determined and result is compensated so that the result that the result that measurement is obtained is obtained closer to the chromatography of ions.
Description of the drawings
Fig. 1 shows the flow chart of the preferred embodiments of the present invention.
Specific embodiment
As shown in figure 1, water quality total phosphorus on-line monitoring method comprises the steps：
(1) sample：200ml water bodys to be measured are gathered by disposable tank；
(2) acid/base ratio is determined：100ml water bodys to be measured are taken, is carried out using the acid solution or sodium hydroxide solution of chlorate anions
Acid-base neutralization；And acid-base value is determined, so as to be calculated the pH value of water body to be measured；
(3) process is shaken up：Disposable tank is at the uniform velocity shaken, and 2ml sodium perchlorate is at the uniform velocity instilled while shake
Solution, treats that instillation is finished, and respectively takes 30ml respectively in two sealable digestion containers, wherein the first digestion container alkali resistance,
Second digestion container acid resistance；
(4) alkalescence is cleared up：Alkaline gas are passed through in the first digestion container, and make the temperature of the first digestion container at 6 points
First degree Celsius is uniformly increased in clock, then, on first degree Celsius 10 minutes is incubated, described first degree Celsius is taken the photograph for 120
Family name degree~200 degree Celsius；
(5) cool down：In 5 minutes, the first digestion container after clearing up cools to 25 degrees Celsius, and in the process to
Neon is passed through in first digestion container；
(6) acidity is cleared up：Sour gas is passed through in the second digestion container, and makes the temperature of the second digestion container at 4 points
Second degree Celsius is uniformly increased in clock, then, on second degree Celsius 12 minutes is incubated, described second degree Celsius is 80 Celsius
~150 degrees Celsius of degree；
(7) cool down：In 5 minutes, the second digestion container after clearing up cools to 25 degrees Celsius, and in the process to
Neon is passed through in second digestion container；
(8) solution in the first digestion container and the second digestion container is settled to into respectively 10ml with distilled water；
(9) in the first digestion container and the second digestion container 3ml ammonium molybdate solutions are separately added into respectively, are sufficiently mixed；
(10) using the digestion container of metric measurement first and the respective total phosphorus content X and Y of the second digestion container；
(11) when the pH value of water body to be measured is more than 7, total phosphorus content=(| | the pH value of water body to be measured | | the * X of water body to be measured
+ (| | the pH value of water body to be measured | |+1) * Y)/(2* | | the pH value of water body to be measured | |)；When the pH value of water body to be measured is less than 7, treat
Total phosphorus content=((| | the pH value of water body to be measured | | -1) * X+ (| | the pH value of water body to be measured | |+1) the * Y) of survey water body/(2* | | treat
Survey the pH value of water body | |).
Further, in the step (2), using the acid solution of chlorate anions acid/base ratio titration is carried out.
Below, more detailed demonstrative example is provided by a specific experiment.
Step 1, sampling.200ml water bodys to be measured are gathered by disposable tank；The disposable tank can be selected
Select disposable plastic bucket or disposable syringe.
Step 2, acid/base ratio is determined：Take 100ml water bodys to be measured to be put in the glass container with inlet and outlet, control
Micro pump adds the hydrochloric acid solution of 0.5mol/L or the sodium hydroxide solution of 0.4mol/L in 100ml water bodys to be measured, with import
The pH value pH1 of solution be reference value, be calculated the difference of the pH value pH2 and pH1 of outlet solution, when difference for bear and less than-
During △ pH, computer controlled automatic micro pump adds alkali liquor in measuring chamber, and soda acid is often added once, the subacid of computer recording one
Dosage or alkali dosage, the △ pH that set in advance are as 0.01~0.05；Every 10~120 seconds, until above-mentioned difference is less than
When set in advance 0.002, stop adding, the accumulative dosage S1 of acid in the time period and accumulative dosage S2 of alkali is calculated, by this
︱ S1-S2 ︱ in time period carry out linear fit, obtain the pH value 5.7 that the corresponding value in line segment midpoint is water body to be measured.
Step 3, shakes up process：Disposable tank is at the uniform velocity shaken using upset well distributing rocker, shake set of time is 5 points
Clock, and 2ml sodium perchlorate solutions are at the uniform velocity instilled while shake, treat that instillation is finished, shake 1 point using upset well distributing rocker again
Clock；30ml is respectively taken respectively in two sealable digestion containers, wherein the first digestion container and the second digestion container are adopted
PVC plastic is made, and with inlet, liquid outlet, air inlet and air vent.This plastics have the excellent of acid resistance and alkali resistance
Point, enables to impact of the measurement result from the unexpected reaction produced during test analysis；
Step 4, alkalescence is cleared up：Alkaline gas are passed through by the air inlet of the first digestion container in the first digestion container,
Air inlet is discharged and be recycled into again to alkaline gas by air vent.Make the temperature of the first digestion container uniform in 6 minutes
120 degrees Celsius are increased to, then, on 120 degrees Celsius 10 minutes are incubated；
Step 5, cooling：In 5 minutes, the first digestion container after being cleared up using spray cooler is cooled to 25 and is taken the photograph
Family name's degree, and neon is passed through in the first digestion container in the process, venting pressure is 2 atmospheric pressure；
Step 6, acidity is cleared up：Sour gas is passed through by the air inlet of the second digestion container in the second digestion container,
Air inlet is discharged and be recycled into again to sour gas by air vent.Make the temperature of the second digestion container uniform in 4 minutes
90 degrees Celsius are increased to, then, on 90 degrees Celsius 12 minutes are incubated；
Step 7, cooling：In 5 minutes, the second digestion container after being cleared up using spray cooler is cooled to 25 and is taken the photograph
Family name's degree, and neon is passed through in the second digestion container in the process, venting pressure is 2 atmospheric pressure；
Step 8,10ml is settled to respectively with distilled water by the solution in the first digestion container and the second digestion container；
Step 9, be sequentially added into in the first digestion container and the second digestion container respectively C6H8O62ml and
H8MoN2O43ml, and be sufficiently mixed after adding every time；
Step 10, using the digestion container of metric measurement first and the respective total phosphorus content 0.53 of the second digestion container
With 0.72；
Step 11, because the pH value of water body to be measured is 5.7, therefore, total phosphorus content=((| | 5.7 | | -1) * of water body to be measured
0.53+ (| | 5.7 | |+1) * 0.72)/(2* | | 5.7 | |)=0.644 (mol/L).
In this test, the total phosphorus value that the chromatography of ions is obtained is adopted for 0.647, it is seen then that this method is obtained using relatively short
Many time has obtained more accurately being worth.
Illustrate the structure of some specific embodiments of the invention in the way of word and description of the drawings above, and it is non-exhaustive
Nothing left is limited to concrete form described above.It should be pointed out that for those skilled in the art, do not taking off
On the premise of the principle of the invention, some improvements and modifications can also be made, these improvements and modifications also should be regarded as the present invention's
Protection domain.
Claims (8)
1. a kind of water quality total phosphorus on-line monitoring method, it is characterised in that comprise the steps：
(1) sample：200ml water bodys to be measured are gathered by disposable tank；
(2) acid/base ratio is determined：Take 100ml water bodys to be measured and determine acid-base value, so as to be calculated the pH value of water body to be measured；
(3) process is shaken up：Disposable tank is at the uniform velocity shaken, and 2ml sodium perchlorate solutions is at the uniform velocity instilled while shake,
Treat that instillation is finished, respectively take 30ml respectively in two sealable digestion containers, wherein the first digestion container alkali resistance, second disappears
Solution container acid resistance；
(4) alkalescence is cleared up：It is passed through alkaline gas in the first digestion container, and makes the temperature of the first digestion container in 6 minutes
First degree Celsius is uniformly increased to, then, on first degree Celsius 10 minutes is incubated；
(5) cool down：In 5 minutes, the first digestion container after clearing up cools to 25 degrees Celsius, and in the process to first
Noble gases are passed through in digestion container；
(6) acidity is cleared up：It is passed through sour gas in the second digestion container, and makes the temperature of the second digestion container in 4 minutes
Second degree Celsius is uniformly increased to, then, on second degree Celsius 12 minutes is incubated；
(7) cool down：In 5 minutes, the second digestion container after clearing up cools to 25 degrees Celsius, and in the process to second
Noble gases are passed through in digestion container；
(8) in the first digestion container and the second digestion container ammonium molybdate solution is separately added into respectively, is sufficiently mixed；
(9) using the digestion container of metric measurement first and the respective total phosphorus content X and Y of the second digestion container；
(10) when the pH value of water body to be measured is more than 7, the total phosphorus content of water body to be measured=(| | the pH value of water body to be measured | | * X+ (| |
The pH value of water body to be measured | |+1) * Y)/(2* | | the pH value of water body to be measured | |)；When the pH value of water body to be measured is less than 7, water to be measured
The total phosphorus content of body=((| | the pH value of water body to be measured | | -1) * X+ (| | the pH value of water body to be measured | |+1) * Y)/(2* | | water to be measured
The pH value of body | |).
2. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that in the step (2), using chlorate anions
Acid solution or sodium hydroxide solution carry out acid/base ratio titration.
3. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that described first degree Celsius is 120 Celsius
~200 degrees Celsius of degree.
4. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that described second degree Celsius is 80 degrees Celsius
~150 degrees Celsius.
5. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that the noble gases are neon.
6. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that also included before step (8)：With steaming
Solution in first digestion container and the second digestion container is settled to respectively 10ml by distilled water.
7. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that the content of the ammonium molybdate solution is
3ml。
8. water quality total phosphorus on-line monitoring method according to claim 1, it is characterised in that before ammonium molybdate solution is added, also plus
Enter ascorbic acid solution.
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| CN201510012716.8A CN104502295B (en) | 2015-01-09 | 2015-01-09 | On-line monitoring method for total phosphorus in water |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112834685A (en) * | 2020-12-31 | 2021-05-25 | 中国环境监测总站 | Method for measuring total phosphorus concentration in surface water |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1137990A (en) * | 1997-07-17 | 1999-02-12 | Toray Eng Co Ltd | Method and instrument for measuring concentration of phosphorus compound in water |
| CN1991339A (en) * | 2005-12-30 | 2007-07-04 | 中国石油化工股份有限公司 | Method for analyzing total phosphorus content in sample |
| CN102998266A (en) * | 2012-11-21 | 2013-03-27 | 合肥星宇化学有限责任公司 | Method for analyzing total phosphorus in industrial sewage sample |
| CN103983597A (en) * | 2014-06-06 | 2014-08-13 | 力合科技（湖南）股份有限公司 | Detection method and system for total nitrogen and total phosphorus |
-
2015
- 2015-01-09 CN CN201510012716.8A patent/CN104502295B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1137990A (en) * | 1997-07-17 | 1999-02-12 | Toray Eng Co Ltd | Method and instrument for measuring concentration of phosphorus compound in water |
| CN1991339A (en) * | 2005-12-30 | 2007-07-04 | 中国石油化工股份有限公司 | Method for analyzing total phosphorus content in sample |
| CN102998266A (en) * | 2012-11-21 | 2013-03-27 | 合肥星宇化学有限责任公司 | Method for analyzing total phosphorus in industrial sewage sample |
| CN103983597A (en) * | 2014-06-06 | 2014-08-13 | 力合科技（湖南）股份有限公司 | Detection method and system for total nitrogen and total phosphorus |
Non-Patent Citations (1)
| Title |
|---|
| 水质总磷的测定 钼酸铵分光光度法;国家环境保护局;《中华人民共和国国家标准》;19900701;第321-324页 * |
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