CN112161970A - Method for determining total phosphorus content in water - Google Patents
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- CN112161970A CN112161970A CN202011005425.3A CN202011005425A CN112161970A CN 112161970 A CN112161970 A CN 112161970A CN 202011005425 A CN202011005425 A CN 202011005425A CN 112161970 A CN112161970 A CN 112161970A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 40
- 239000011574 phosphorus Substances 0.000 title claims abstract description 40
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 13
- 230000029087 digestion Effects 0.000 claims abstract description 13
- 238000004993 emission spectroscopy Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 6
- 239000000779 smoke Substances 0.000 claims description 6
- 238000000295 emission spectrum Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 10
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000011161 development Methods 0.000 abstract description 7
- 229910052785 arsenic Inorganic materials 0.000 abstract description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 239000011651 chromium Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 30
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- 238000002798 spectrophotometry method Methods 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- 239000011609 ammonium molybdate Substances 0.000 description 7
- 229940010552 ammonium molybdate Drugs 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 5
- 235000018660 ammonium molybdate Nutrition 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000011964 heteropoly acid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- HSNVNALJRSJDHT-UHFFFAOYSA-N P(=O)(=O)[Mo] Chemical compound P(=O)(=O)[Mo] HSNVNALJRSJDHT-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001462 antimony Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012925 reference material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
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Abstract
The invention relates to the technical field of phosphorus content detection, in particular to a method for determining total phosphorus content in water. The method comprises the following steps: digesting a water sample to be detected by using mixed acid; the mixed acid is sulfuric acid and perchloric acid which are mixed in equal proportion. The method for performing the measurement is inductively coupled plasma emission spectrometry. Through experiments, a common water sample can be completely digested by adding a small amount of sulfuric acid and perchloric acid in equal proportion, the pH value is not required to be adjusted after digestion is finished, and color development is not required in the determination process; when the inductively coupled plasma emission spectrometer is used for measurement, the inductively coupled plasma emission spectrometer is not influenced by elements such as arsenic, sulfide and chromium, is not limited by color development time, is not influenced by room temperature, improves the test efficiency, increases the test precision, and is more suitable for testing large batches of samples in a laboratory.
Description
Technical Field
The invention relates to the technical field of phosphorus content detection, in particular to a method for determining total phosphorus content in water.
Background
At present, methods for measuring total phosphorus in water comprise methods such as GB 11893-1989 ammonium molybdate spectrophotometry for measuring total phosphorus in water, HJ 670-2013 continuous flow-ammonium molybdate spectrophotometry for measuring phosphate and total phosphorus in water, HJ 671-2013 flow injection-ammonium molybdate spectrophotometry for measuring total phosphorus in water, MT/T743.1-2011 method for measuring total phosphorus in coal mine water, and the like.
The method adopts an ammonium molybdate spectrophotometry or a phosphomolybdenum blue spectrophotometry, needs to prepare a color developing agent and a buffering agent, has strict time requirement, and influences the measurement result of the total phosphorus content in the sample if the reaction time of a standard curve and the sample is inconsistent. And when the sample amount is large, the method is limited by conditions such as time, equipment, personnel and the like, the efficiency is low, and the method is not beneficial to batch laboratory inspection and detection.
Taking GB 11893-1989 ammonium molybdate spectrophotometry for measuring total phosphorus in water as an example, the principle is as follows: the sample is digested by potassium persulfate under neutral condition, all the phosphorus contained is oxidized into orthophosphate, the orthophosphate reacts with ammonium molybdate in an acidic medium, and after phosphomolybdic heteropoly acid is produced in the presence of antimony salt, the phosphomolybdic heteropoly acid is immediately reduced by ascorbic acid to generate blue complex. The method is a classical laboratory method and is widely used, but has some defects:
(1) the water quality sample needs to be added with sulfuric acid to adjust the pH value for storage during collection, so that the sample needs to be adjusted to be neutral firstly when potassium persulfate is used for digestion.
(2) If the turbidity or the color is contained in the sample, a blank sample is prepared, then 3mL of turbidity-color compensation solution is added to the sample without adding ascorbic acid and molybdate, and then the absorbance of the blank sample is subtracted from the absorbance of the sample.
(3) When the arsenic is more than 2mg/L, the measurement is interfered, and sodium thiosulfate is used for removing the arsenic; when the sulfide is more than 2mg/L, the measurement is interfered, and nitrogen is needed to be introduced for removal; chromium above 50mg/L interferes with the assay and is removed with sodium sulfite.
(4) If the room temperature is lower than 13 ℃ during color development, heating and color development for 15min on a water bath at the temperature of 20-30 ℃ are needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for measuring the total phosphorus content in water.
Specifically, the method for determining the total phosphorus content in water comprises the following steps: digesting a water sample to be detected by using mixed acid;
the mixed acid is sulfuric acid and perchloric acid which are mixed in equal proportion.
The invention unexpectedly discovers that the method is favorable for destroying organic matters and dissolving suspended matters by digesting the water sample to be detected by adopting the sulfuric acid and the perchloric acid which are mixed in equal proportion, and dissolving out phosphorus in various forms in the sample so as to be convenient for determination.
In the invention, the sulfuric acid is commercially available concentrated sulfuric acid, and the perchloric acid is commercially available concentrated perchloric acid.
Preferably, the measurement is performed by inductively coupled plasma emission spectroscopy.
According to the invention, the method is adopted to determine the digested water sample, so that the method has the advantages of less interference, large linear range, small error of determination result and simplicity and convenience in operation.
Preferably, the volume ratio of the water sample to be detected to the mixed acid is 20-30: 2 to 4. The water sample to be detected is cleared up according to the volume ratio, and organic matters and suspended matters are more favorably destroyed and dissolved.
Preferably, the digestion is: adding the mixed acid into a water sample to be detected, uniformly mixing, heating to 220-250 ℃, digesting until white smoke is emitted, adjusting the heating temperature to 180-200 ℃, refluxing until the residual liquid is colorless, and cooling and fixing the volume.
In the technical scheme, if the residual liquid has a color, the mixed acid can be added again to continue heating until the residual liquid is clear, transparent and free of precipitate.
Preferably, the method for determining the total phosphorus content in water comprises the following steps:
(1) digestion: adding 2-4 mL of mixed acid into 20-30 mL of water sample to be detected, uniformly mixing, heating to 220-250 ℃, digesting until white smoke is emitted, adjusting the heating temperature to 180-200 ℃, refluxing until the residual liquid is colorless, cooling, and fixing the volume with water to obtain a sample to be detected; the volume ratio of the residual liquid to the constant volume is 3-4: 50;
(2) and (3) measuring by adopting an inductively coupled plasma emission spectrometry: and (3) preparing a working curve by using series of standard solutions with different concentrations, detecting the inductively coupled plasma emission spectrum of the sample to be detected, and obtaining the total phosphorus content according to the working curve.
In the above technical scheme, a standard solution can be prepared by using a commercial phosphorus standard solution or a potassium dihydrogen phosphate standard substance.
Preferably, in the step (2), the wavelength of the emission spectrum of the inductively coupled plasma is 214.914 nm.
Preferably, in the step (2), the power is 1150W, the pump speed is 40rpm, the vertical observation height is 12mm, the cooling air flow rate is 1.0L/min, the atomizer pressure is 0.3MPa, and the integration time is 2 s.
Preferably, in the step (2), a series of standard solutions with the concentration of 0.1-100 mug/mL are adopted, and the concentration gradient is 0.1-10 mug/mL.
The invention has the beneficial effects that:
(1) through experiments, a common water sample can be completely digested by adding a small amount of sulfuric acid and perchloric acid in equal proportion; the improvement can save reagent dosage, save cost and reduce environmental pollution.
(2) After digestion, pH value does not need to be adjusted, reagents such as phenolphthalein, sodium hydroxide, sulfuric acid and the like are not used, the use of the reagents is reduced, the cost of the reagents is saved, and the pollution to the environment is reduced.
(3) The color development is not needed in the determination process, and reagents such as ascorbic acid, molybdate and the like are not used, so that the use of the reagents is reduced, the cost is saved, and the environmental pollution is reduced.
(4) When the inductively coupled plasma emission spectrometer is used for measurement, the inductively coupled plasma emission spectrometer is not influenced by elements such as arsenic, sulfide and chromium, and is not required to be removed or masked by adding a reagent, so that the operation steps are saved, the use of the reagent is reduced, the cost is saved, and the environmental pollution is reduced.
(5) Compared with the measurement of a spectrophotometer, the measurement of the inductively coupled plasma emission spectrometer improves the test efficiency, increases the test precision, and is suitable for the test of a large number of samples in a laboratory.
(6) The measurement by using the inductively coupled plasma emission spectrometry is not limited by the color development time and is not influenced by room temperature, so that the method is more suitable for testing a large number of samples in a laboratory.
Drawings
FIG. 1 is a working curve of example 1.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the examples, unless otherwise specified, the methods used are conventional in the art.
The instruments and reagents involved in the examples are as follows:
inductively coupled plasma emission spectrometer: iCAP-6300, available from American thermoelectric corporation (Saimer Feishale);
sulfuric acid: commercial concentrated sulfuric acid super-grade purity;
perchloric acid: the commercial concentrated perchloric acid is superior pure;
nitric acid: the concentrated nitric acid sold in the market is superior pure;
phosphorus standard stock solution: the reference material was prepared from commercially available potassium dihydrogen phosphate.
Example 1
The embodiment provides a method for measuring the total phosphorus content in water, which comprises the following steps:
(1) digestion: putting 25mL of water sample to be detected into a 100mL beaker, adding 1mL of sulfuric acid and 1mL of perchloric acid, covering a surface dish, shaking uniformly, placing on an electric heating plate, heating to 220-250 ℃ for digestion, digesting until white smoke is emitted, adjusting the temperature of the electric heating plate to 180-200 ℃ to keep the digestion solution in a reflux state in the beaker until 3-4 mL of liquid is left and the solution is colorless, and taking down. After cooling, the volume is determined to be 50mL volumetric flask, the volume is determined to be the water volume, and the shaking is carried out uniformly.
(2) Measuring by using an inductively coupled plasma emission spectrometer, wherein the wavelength is 214.914 nm; the power was 1150W, the pump speed was 40rpm, the vertical observation height was 12mm, the cooling gas flow was 1.0L/min, the atomizer pressure was 0.3MPa, and the integration time was 2 s.
And (3) preparing a working curve (as shown in figure 1) by using a series of phosphorus standard solutions with different concentrations, detecting the inductively coupled plasma emission spectrum of the sample to be detected, and obtaining the total phosphorus content according to the working curve.
Comparative example 1
This comparative example provides a method for determining the total phosphorus content in water, differing from example 1 only in that: and (3) digesting the water sample to be detected by adopting 2mL of nitric acid in the step (1).
Comparative example 2 spectrophotometric determination of total phosphorus content
The method is an ammonium molybdate spectrophotometry for measuring total phosphorus in water quality in GB 11893-1989, and the method comprises the following specific operation steps:
(1) digestion: the method comprises the following steps: taking 25mL of water sample, putting the water sample into a 50mL colorimetric tube, adding potassium persulfate, sealing, heating until the pressure reaches 1.1kg/cm3Keeping the temperature at 120 ℃ for 30min, and then stopping heating. Taking out the pressure gauge after the reading of the pressure gauge is 0, cooling the pressure gauge, and diluting the pressure gauge to a scale;
the second method comprises the following steps: taking 25mL of water sample into a conical flask, adding a plurality of glass beads, adding 2mL of concentrated nitric acid, heating and concentrating on an electric hot plate to 10mL, cooling, adding 5mL of concentrated nitric acid, heating and concentrating to 10mL, and cooling. Adding 3mL of concentrated perchloric acid, heating until white smoke is emitted, adjusting the temperature of an electric heating plate or adding a small funnel to keep the digestion solution in a reflux state in a conical flask until 3-4 mL of digestion solution is left, and cooling. Adding 10mL of water and 1 drop of phenolphthalein, using sodium hydroxide to modulate the mixture to be just reddish, then dropping sulfuric acid to just fade the red, shaking the mixture evenly, transferring the mixture into a 50mL colorimetric tube, and diluting the mixture to a marked line by using water.
(2) Color development: 1mL of ascorbic acid was added to each solution and mixed well, and after 30s, 2mL of molybdate solution was added and mixed well.
(3) Spectrophotometric measurement: and standing at room temperature for 15min, measuring absorbance by using a cuvette with an optical path of 30mm and taking water as a reference at the wavelength of 700nm, deducting the absorbance of a blank test, and checking the content of phosphorus from a working curve.
Experimental example 1
In the experimental example, the method for measuring the total phosphorus content in water provided in example 1 and comparative examples 1 to 2 is considered, and specifically, the method comprises the following steps:
(1) preparing a water sample to be detected: weighing 0.439g of monopotassium phosphate, dissolving the monopotassium phosphate in water, transferring the monopotassium phosphate into a 1000mL volumetric flask for dilution to scale to obtain phosphorus standard stock with the concentration of 0.1 mg/mL; then 10mL of phosphorus standard stock solution is dispensed into a 100mL volumetric flask and diluted to a scale, so as to obtain a water sample to be detected; the total phosphorus content in the obtained water sample to be detected is 10 mu g/mL.
(2) The method of example 1 and the method of comparative examples 1-2 are respectively adopted to determine the water sample to be measured, and the determination results are shown in table 1;
TABLE 1
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. A method for determining the total phosphorus content in water, comprising: digesting a water sample to be detected by using mixed acid;
the mixed acid is sulfuric acid and perchloric acid which are mixed in equal proportion.
2. The method of claim 1, wherein the method of measuring is inductively coupled plasma emission spectroscopy.
3. The method for determining the total phosphorus content in water according to claim 1, wherein the volume ratio of the water sample to be tested to the mixed acid is 20-30: 2 to 4.
4. The method for determining the total phosphorus content in water according to claim 1 or 3, wherein the digestion is: adding the mixed acid into a water sample to be detected, uniformly mixing, heating to 220-250 ℃, digesting until white smoke is emitted, adjusting the heating temperature to 180-200 ℃, refluxing until the residual liquid is colorless, and cooling and fixing the volume.
5. The method for determining the total phosphorus content in water according to any one of claims 1 to 4, comprising the steps of:
(1) digestion: adding 2-4 mL of mixed acid into 20-30 mL of water sample to be detected, uniformly mixing, heating to 220-250 ℃, digesting until white smoke is emitted, adjusting the heating temperature to 180-200 ℃, refluxing until the residual liquid is colorless, cooling, and fixing the volume with water to obtain a sample to be detected; the volume ratio of the residual liquid to the constant volume is 3-4: 50;
(2) and (3) measuring by adopting an inductively coupled plasma emission spectrometry: and (3) preparing a working curve by using series of standard solutions with different concentrations, detecting the inductively coupled plasma emission spectrum of the sample to be detected, and obtaining the total phosphorus content according to the working curve.
6. The method for determining the total phosphorus content in water as claimed in claim 5, wherein in the step (2), the wavelength of the emission spectrum of the inductively coupled plasma is 214.914 nm.
7. The method for measuring the total phosphorus content in water as claimed in claim 5, wherein in the step (2), the power is 1150W, the pump speed is 40rpm, the vertical observation height is 12mm, the cooling air flow rate is 1.0L/min, the atomizer pressure is 0.3MPa, and the integration time is 2 s.
8. The method for determining the total phosphorus content in water according to claim 5, wherein in the step (2), a series of standard solutions with the concentration of 0.1-100 μ g/mL are adopted, and the concentration gradient is 0.1-10 μ g/mL.
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| JPH08285834A (en) * | 1995-04-13 | 1996-11-01 | Yokogawa Electric Corp | Continuous water quality measuring system |
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|---|---|---|---|---|
| CN86210497U (en) * | 1986-12-16 | 1987-12-12 | 郑光倩 | Automatical trace organism transforming device under dynamic burning in water |
| JPH08285834A (en) * | 1995-04-13 | 1996-11-01 | Yokogawa Electric Corp | Continuous water quality measuring system |
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