CN113884450A - Turbidity chromaticity correction method for automatic water quality monitor - Google Patents
Turbidity chromaticity correction method for automatic water quality monitor Download PDFInfo
- Publication number
- CN113884450A CN113884450A CN202111083329.5A CN202111083329A CN113884450A CN 113884450 A CN113884450 A CN 113884450A CN 202111083329 A CN202111083329 A CN 202111083329A CN 113884450 A CN113884450 A CN 113884450A
- Authority
- CN
- China
- Prior art keywords
- absorbance
- water sample
- water
- solution
- detected
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 238000012937 correction Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002835 absorbance Methods 0.000 claims abstract description 82
- 238000011161 development Methods 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000012544 monitoring process Methods 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 84
- 239000012086 standard solution Substances 0.000 claims description 34
- 230000029087 digestion Effects 0.000 claims description 17
- 238000001514 detection method Methods 0.000 abstract description 12
- 238000002798 spectrophotometry method Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000010998 test method Methods 0.000 abstract description 3
- 238000004737 colorimetric analysis Methods 0.000 abstract 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 46
- 239000012498 ultrapure water Substances 0.000 description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 24
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 24
- 229910052802 copper Inorganic materials 0.000 description 24
- 239000010949 copper Substances 0.000 description 24
- 238000005259 measurement Methods 0.000 description 23
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 22
- 229910052698 phosphorus Inorganic materials 0.000 description 22
- 239000011574 phosphorus Substances 0.000 description 22
- 229910052759 nickel Inorganic materials 0.000 description 21
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 18
- 238000010561 standard procedure Methods 0.000 description 15
- 239000000843 powder Substances 0.000 description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 12
- 238000007865 diluting Methods 0.000 description 11
- 238000005303 weighing Methods 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 229960005070 ascorbic acid Drugs 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 239000005708 Sodium hypochlorite Substances 0.000 description 8
- LMBWSYZSUOEYSN-UHFFFAOYSA-N diethyldithiocarbamic acid Chemical compound CCN(CC)C(S)=S LMBWSYZSUOEYSN-UHFFFAOYSA-N 0.000 description 8
- 229950004394 ditiocarb Drugs 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 239000011550 stock solution Substances 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 6
- -1 sodium nitrosoferricyanide Chemical compound 0.000 description 6
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 5
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 5
- 239000002211 L-ascorbic acid Substances 0.000 description 5
- 235000000069 L-ascorbic acid Nutrition 0.000 description 5
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 5
- 238000005189 flocculation Methods 0.000 description 5
- 230000016615 flocculation Effects 0.000 description 5
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 5
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RGJFLQSCKQTTRF-UHFFFAOYSA-L C(=O)([O-])C(O)C(O)C(=O)[O-].[Na+].[K+].C(C=1C(O)=CC=CC1)(=O)O Chemical compound C(=O)([O-])C(O)C(O)C(=O)[O-].[Na+].[K+].C(C=1C(O)=CC=CC1)(=O)O RGJFLQSCKQTTRF-UHFFFAOYSA-L 0.000 description 4
- 229940026189 antimony potassium tartrate Drugs 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 description 4
- WBTCZEPSIIFINA-MSFWTACDSA-J dipotassium;antimony(3+);(2r,3r)-2,3-dioxidobutanedioate;trihydrate Chemical compound O.O.O.[K+].[K+].[Sb+3].[Sb+3].[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O.[O-]C(=O)[C@H]([O-])[C@@H]([O-])C([O-])=O WBTCZEPSIIFINA-MSFWTACDSA-J 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 235000018660 ammonium molybdate Nutrition 0.000 description 3
- 239000011609 ammonium molybdate Substances 0.000 description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 3
- 229940010552 ammonium molybdate Drugs 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000001476 sodium potassium tartrate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
Landscapes
- 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 turbidity chromaticity correction method for an automatic water quality monitor, and belongs to the technical field of water quality detection. When the absorbance of a water sample is measured by colorimetry, firstly measuring the absorbance A1 of the water sample to be measured before color development, adding a color developing agent, then measuring the absorbance A2 of the water sample to be measured after the color developing agent is added, simultaneously recording the volumes V1 and V2 of the water sample to be measured before and after the color developing agent is added, correcting the absorbance before color development according to the inverse relation between the absorbance and the volume of the water sample to be measured, wherein the correction formula is A1 ═ A1 ═ (V1/V2), taking the difference between A2 and A1 ', namely Δ A ═ A2-A1' as the absorbance A after correction of a reaction system, and finally calculating the concentration of a corresponding index according to a standard curve. The turbidity chromaticity correction is realized when the water quality parameter based on the color reaction is measured by the spectrophotometry. The test method has simple and convenient operation steps, and does not need to pretreat the water sample; the test result has high accuracy, high efficiency and short time consumption; the method is suitable for being applied to automatic monitoring instruments, and extra cost is not increased.
Description
Technical Field
The invention relates to a turbidity chromaticity correction method for an automatic water quality monitor, and belongs to the technical field of water quality detection.
Background
The automatic water quality monitor is an on-line analyzer capable of automatic sampling and quantitative analysis, and is widely used for on-line automatic monitoring of surface water and sewage, and mainly comprises automatic water quality monitors of total nitrogen, ammonia nitrogen, chemical oxygen demand, total phosphorus, heavy metals and the like. The detection of these parameters is mostly based on the chromogenic reaction of the substance to be detected with a specific chromogenic agent, and is carried out quantitatively by spectrophotometry. However, the actual water sample itself may have a certain degree of turbidity and chromaticity, which may cause a great interference to the accuracy of water quality detection based on spectrophotometry.
In order to eliminate the influence of the turbidity and the chromaticity of a water sample on a detection result, the method for correcting the turbidity and the chromaticity in the national standard method mainly comprises flocculation precipitation, distillation, digestion, chromaticity-turbidity compensation liquid and the like. Liurongwei (CN107782681A) uses a chromaticity-turbidity compensation solution and a flocculation precipitation method to pretreat a water sample and then measure hexavalent chromium, although the detection accuracy is improved, the operation steps are complicated, and redundant reagents and time are consumed; the Zhangliang (CN109187388A) uses a method of chroma-turbidity compensation liquid to replace a flocculation precipitation and distillation method specified in an ammonia nitrogen national standard method, improves the ammonia nitrogen detection efficiency of the liquor industrial wastewater, but does not fundamentally solve the problems of complex operation and redundant reagent consumption. It is clear that these methods either require complex reagents or require complex equipment, and that the addition of these pre-treatment units significantly increases the manufacturing costs of the water quality automatic monitor. Most of pretreatment devices of the automatic water quality monitor are filtering/settling, the methods are relatively simple and easy to realize, large-particle substances in a water sample can be removed, and the interference of the turbidity and the chromaticity of the water sample on measurement cannot be completely solved.
The interference of turbidity chromaticity on the detection of water quality parameters is mainly because particles in a water sample or the color of the water sample has certain absorbance, and for parameters such as total phosphorus, total nitrogen, total nickel and the like which need to measure the total amount of pollutants in the water sample, the water sample needs to be digested at high temperature before measurement, although the interference of the turbidity of the water sample can be obviously reduced in the process, the removal of the chromaticity is still limited; for the water quality parameters such as ammonia nitrogen, high-temperature digestion is not needed before testing, so that the interference of turbidity and chromaticity of the water sample is more obvious. Therefore, the method takes the absorbance of the background of the water sample (or the digested water sample) as blank, and realizes the deduction of the turbidity and the chromaticity of the water sample by correcting the change of the volume of the solution caused by adding the color developing agent, thereby carrying out accurate automatic detection on the water quality parameters.
Disclosure of Invention
The invention aims to overcome the defects of the prior water sample turbidity and chromaticity preprocessing means, provides a turbidity and chromaticity correction method for automatic water quality monitoring, and realizes turbidity and chromaticity correction when water quality parameters are measured by a spectrophotometry.
In order to achieve the purpose, the invention adopts the technical scheme that: a turbidity chromaticity correction method for automatic water quality monitoring comprises the following steps:
(1) drawing a standard curve: preparing a series of standard solutions with different concentrations, testing the absorbance of the solutions in a spectrophotometer/automatic monitoring equipment after digestion, and establishing a standard curve to obtain a linear relation equation of the concentration of the standard solution and the absorbance of the standard solution;
(2) and (3) determining a sample: taking pure water as reference, determining the absorbance A1 of the water sample to be detected before color development, adding a color developing agent, determining the absorbance A2 of the water sample to be detected after color development, and recording the volume V1 of the water sample to be detected before color development and the volume V2 of the water sample to be detected after color development;
(3) and (3) correcting the absorbance value: correcting the absorbance A1 before the color development of the water sample to be detected according to the volume V1 when A1 is measured and the volume V2 when A2 is measured, wherein the correction formula is as follows: a 1' ═ a1 (V1/V2);
(4) and (3) calculating the concentration: and (3) substituting the absorbance A of the obtained water sample to be detected into the standard curve in the step (1) to calculate the concentration of the water sample to be detected, wherein the difference value of the absorbance A2 of the water sample to be detected after color development and the absorbance A1' of the water sample to be detected before color development after correction is the absorbance A of the water sample to be detected.
In the water sample detection process, the absorbance A1 before and after the solution is developed and the absorbance A2 after the solution is developed are measured, the volumes V1 and V2 before and after the solution is developed are recorded at the same time, the absorbance before the development is corrected according to the inverse relation between the absorbance and the solution volume, the correction formula is A1 ═ A1 (V1/V2), the difference between A2 and A1 ', namely delta A ═ A2-A1', is used as the absorbance A (delta A ═ A) after the reaction system is corrected, and finally, the concentration of the corresponding index is calculated according to a standard curve. The turbidity and chromaticity correction during the determination of the water quality parameters such as total copper, total nickel, total phosphorus, ammonia nitrogen and the like by a spectrophotometry method is realized. The method overcomes the defect that the water sample pretreatment technologies such as flocculation precipitation, distillation and digestion are not easy to realize on an automatic monitoring instrument in the prior art, improves the accuracy of the measurement result, is simple to operate, avoids complex pretreatment steps, does not need to use redundant reagents, can be widely applied to the turbidity and chromaticity correction of high-turbidity and chromaticity water samples in the water quality parameter detection process by taking a color development-spectrophotometry method as a detection means, and is suitable for being applied to automatic monitoring equipment.
As a preferred embodiment of the turbidity chromaticity correction method for automatically monitoring water quality, the standard working curve obtained in the step (1) is as follows: k x + b
Wherein y is the absorbance of the standard solution, x is the concentration of the standard solution, k is the slope coefficient of the reticle, and b is the intercept coefficient of the reticle.
Compared with the prior art, the invention has the beneficial effects that:
1. the test method disclosed by the invention is simple and convenient in operation steps, a water sample is not required to be pretreated, and no redundant reagent is consumed;
2. the test method is suitable for being applied to automatic monitoring instruments, does not increase extra cost, and only needs to correct data.
3. The invention has the advantages of high accuracy of test results, high efficiency and short time consumption.
Drawings
FIG. 1 is a standard curve of total nickel concentration versus absorbance for a standard solution;
FIG. 2 is a standard curve of total copper concentration versus absorbance for a standard solution;
FIG. 3 is a standard curve of total phosphorus concentration versus absorbance for a standard solution;
FIG. 4 is a standard curve of ammonia nitrogen concentration and absorbance of a standard solution.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
Example 1
The embodiment provides a total nickel turbidity chromaticity correction method for automatic water quality monitoring, which comprises the following steps:
1. preparation of the solution
The preparation method of the nickel standard solution comprises the following steps:
1) accurately weighing 0.1000g of metallic nickel (the content is more than 99.9%), dissolving the metallic nickel in 10mL of (1+1) nitric acid solution, heating and evaporating the solution to be nearly dry, cooling the solution, adding the (1+99) nitric acid solution to dissolve the solution, transferring the solution into a 100mL volumetric flask, and diluting the solution with ultrapure water to a marked line to obtain 1000mg/L nickel standard stock solution.
2) Accurately transferring 2mL of 1000mg/L nickel standard stock solution into a 100mL volumetric flask, metering the volume to the marked line by using ultrapure water, and shaking up to obtain the nickel standard intermediate solution with the concentration of 20 mg/L.
3) Accurately transferring 0.1mL, 0.5mL, 2.5mL, 5.0mL, 12.5mL and 25.0mL of the nickel standard intermediate solution with the concentration of 20mg/L into a 50mL volumetric flask, fixing the volume to the marked line by using ultrapure water, and shaking up to obtain nickel standard solutions with the concentrations of 0.04mg/L, 0.2mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L and 10.0mg/L respectively.
The oxidant preparation steps are as follows:
weighing 5.0g of ammonium persulfate powder into a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring into a 100mL volumetric flask, and diluting with ultrapure water to a marked line to obtain 50g/L of ammonium persulfate solution.
The masking agent is formulated as follows:
weighing 9.0g of potassium sodium tartrate powder into a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring into a 100mL volumetric flask, and diluting with ultrapure water to a marked line to obtain 90g/L potassium sodium tartrate solution.
The color developing agent is prepared by the following steps:
0.5g of dimethylglyoxime powder and 10.0g of sodium hydroxide solid are respectively weighed and put into a 100mL beaker, about 60mL of ultrapure water is added, the mixture is stirred by a glass rod until the mixture is completely dissolved, the mixture is transferred into a 100mL volumetric flask and diluted to a marked line by the ultrapure water, and then the mixed solution of 5g/L dimethylglyoxime and 100g/L sodium hydroxide is obtained.
2. Drawing a working curve
Putting 5.0mL of nickel standard solutions with the concentrations of 0.04mg/L, 0.20mg/L, 1.00mg/L, 2.00mg/L, 5.00mg/L and 10.00mg/L into a 10mL digestion tube respectively, adding 0.3mL of 50g/L ammonium persulfate, sealing, heating at 121 ℃ for 10min, taking out, cooling to room temperature by using tap water, adding 0.6mL of 90g/L potassium sodium tartrate, adding 0.7mL of 50g/L ammonium persulfate, mixing uniformly, standing for 2min, adding 0.7mL of a mixed solution of 5g/L dimethylglyoxime and 100g/L sodium hydroxide, standing for 10min, and determining the absorbance A of the standard solution by using pure water as a reference at 470 nm. And (4) drawing a standard curve by taking the concentration of nickel as an abscissa and the corresponding absorbance as an ordinate. The equation is that y is 0.2167x +0.0049, the linear range of the total nickel is 0-10 mg/L, and the correlation coefficient r2＝0.9999。
In this example, the standard curve of total nickel concentration versus absorbance for the standard solution is shown in table 1 and fig. 1.
TABLE 1 Standard Curve of Total Nickel concentration versus Absorbance of Standard solutions
3. Determination of water sample to be measured
Taking 5.0mL of a water sample to be detected, putting the water sample into a 10mL digestion tube, adding 0.3mL of 50g/L ammonium persulfate, digesting the water sample for 10min at 121 ℃, cooling, adding 0.6mL of 90g/L potassium sodium tartrate, adding 0.7mL of 50g/L ammonium persulfate, uniformly mixing, standing for 2min, taking pure water as reference at a wavelength of 470nm, determining the absorbance A1 of the water sample before color development, finally adding 0.7mL of a mixed solution of 5g/L dimethylglyoxime and 100g/L sodium hydroxide, standing for 10min, taking pure water as reference at 470nm, determining the absorbance A2 of the water sample after color development, obtaining the absorbance A of the water sample to be detected through correction, and calculating the total nickel concentration of the water sample to be detected according to a standard curve.
And (3) correction of the absorbance value: the absorbance a1 was corrected based on the volume V1 at the time of measurement of a1 and the volume V2 at the time of measurement of a2, i.e., a1 ═ a1 (V1/V2), and the difference between a2 and a1 ', i.e., Δ a ═ a2-a 1', was used as the absorbance a of the sample after correction.
4. Testing the total nickel concentration of the water sample to be tested by the national standard method
Taking 5.0mL of water sample to be detected, putting the water sample into a 10mL digestion tube, adding 0.3mL of 50g/L ammonium persulfate, digesting the water sample at 121 ℃ for 10min, and after the water sample is digested, using a microwave plasma atomic emission spectrometer to determine the total nickel concentration of the water sample to be detected.
5. Test results
The total nickel concentration in water samples of different turbidity chromaticities was determined using the method of this example and the national standard method, and the test results are shown in table 2.
TABLE 2
As can be seen from Table 2, the measurement results of two different water samples which do not pass turbidity chromaticity correction have larger difference with the test results of the national standard method, and the relative errors are 83.26 percent and 18.12 percent respectively; after turbidity chromaticity correction, the total nickel concentration of the measured water sample is close to the value measured by the national standard method, and the relative errors are-0.36 percent and-4.12 percent respectively. The method for correcting the total nickel turbidity chromaticity is effective in the measurement of the actual water sample and has high accuracy.
Example 2
The embodiment provides a total copper turbidity chromaticity correction method for automatic water quality monitoring, which comprises the following steps:
1. preparation of the solution
The preparation method of the copper standard solution comprises the following steps:
1) accurately weighing 0.2000g of metal copper (with the content of more than 99.9 percent), placing the metal copper into a 250mL conical flask, adding 20.0mL of ultrapure water and 10.0mL of (1+1) nitric acid solution, heating for dissolving until the reaction speed is slowed down, slightly heating to dissolve all copper, boiling the solution to remove nitrogen oxide, cooling, adding the ultrapure water for dissolving, transferring the solution into a 1000mL volumetric flask, and diluting the solution to a marked line by using the ultrapure water to obtain 200mg/L copper standard stock solution.
2) Accurately transferring 10.0mL of 200mg/L copper standard stock solution into a 100mL volumetric flask, metering the volume to the marked line by using ultrapure water, and shaking up to obtain the copper standard intermediate solution with the concentration of 20 mg/L.
3) Accurately transferring 0.125mL, 0.25mL, 0.5mL, 1.25mL, 5.0mL and 12.5mL of the copper standard intermediate solution with the concentration of 20mg/L respectively, placing the copper standard intermediate solution into a 50mL volumetric flask, fixing the volume to a marked line by using ultrapure water, and shaking up to obtain copper standard solutions with the concentrations of 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 2.00mg/L and 5.00mg/L respectively.
The oxidant preparation steps are as follows:
weighing 5.0g of ammonium persulfate powder into a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring into a 100mL volumetric flask, and diluting with ultrapure water to a marked line to obtain 50g/L of ammonium persulfate solution.
The masking agent is formulated as follows:
respectively weighing 5.0g of disodium ethylene diamine tetraacetate powder and 20.0g of ammonium citrate solid in a 100mL beaker, adding 80.0mL of ultrapure water, stirring by a glass rod until the disodium ethylene diamine tetraacetate powder and the ammonium citrate solid are completely dissolved, transferring the mixture into a 100mL volumetric flask, and diluting the mixture with the ultrapure water until the mixture is marked, thus obtaining a mixed solution of 50g/L disodium ethylene diamine tetraacetate and 200g/L ammonium citrate.
Weighing 9.0g of sodium hydroxide solid into a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring into a 100mL volumetric flask, and diluting with ultrapure water to a marked line to obtain 90g/L of sodium hydroxide solution.
The color developing agent is prepared by the following steps:
weighing 0.2g of sodium diethyldithiocarbamate powder into a 100mL beaker, adding a small amount of ultrapure water to dissolve the sodium diethyldithiocarbamate powder completely, transferring the sodium diethyldithiocarbamate powder into a 100mL volumetric flask, diluting the sodium diethyldithiocarbamate powder with the ultrapure water to a marked line to obtain 2g/L of sodium diethyldithiocarbamate solution, and storing the sodium diethyldithiocarbamate solution in a brown bottle in a dark place for two weeks.
2. Drawing a working curve
Putting 4.0mL of copper standard solutions with concentrations of 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 2.00mg/L and 5.00mg/L into a 10mL digestion tube respectively, adding 0.5mL of 50g/L ammonium persulfate, sealing, heating at 121 ℃ for 10min, taking out, cooling to room temperature by using tap water, adding a mixed solution of 1.0mL of 50g/L disodium ethylenediamine tetraacetate and 200g/L ammonium citrate, adding 0.5mL of 90g/L sodium hydroxide solution, uniformly mixing, finally adding 0.5mL of 2g/L sodium diethyldithiocarbamate, shaking uniformly, and immediately determining absorbance A by using pure water as a reference at 440 nm. And drawing a standard curve by taking the concentration of copper as an abscissa and the corresponding absorbance as an ordinate. The equation is that y is 0.1288x +0.0059, the linear range of total copper is 0-5 mg/L, and the correlation coefficient r2＝0.9994。
In this example, the standard curve of total copper concentration versus absorbance for the standard solution is shown in table 3 and fig. 2.
TABLE 3 Standard Curve of Total copper concentration versus Absorbance of Standard solutions
3. Determination of water sample to be measured
Taking 4.0mL of a water sample to be detected into a 10mL digestion tube, adding 0.5mL of 50g/L ammonium persulfate, sealing, digesting at 121 ℃ for 10min, cooling, adding 1.0mL of a mixed solution of 50g/L disodium ethylenediamine tetraacetate and 200g/L ammonium citrate, adding 0.5mL of 90g/L sodium hydroxide, uniformly mixing, performing reference determination by pure water at the wavelength of 440nm, and determining the absorbance A1 of the water sample to be detected before color development, finally adding 0.5mL of 2g/L sodium diethyldithiocarbamate, shaking uniformly, immediately performing reference by pure water at the wavelength of 440nm, determining the absorbance A2 of the water sample to be detected after color development, obtaining the absorbance A of the water sample to be detected through correction, and calculating the total copper concentration of the water sample to be detected according to a standard curve.
And (3) correction of the absorbance value: the absorbance a1 was corrected based on the volume V1 at the time of measurement of a1 and the volume V2 at the time of measurement of a2, i.e., a1 ═ a1 (V1/V2), and the difference between a2 and a1 ', i.e., Δ a ═ a2-a 1', was used as the absorbance a of the sample after correction.
4. Testing the total copper concentration of the water sample to be tested by the national standard method
Taking 4.0mL of water sample to be detected, putting the water sample into a 10mL digestion tube, adding 0.5mL of 50g/L ammonium persulfate, sealing, digesting for 10min at 121 ℃, and after the water sample is digested, using a microwave plasma atomic emission spectrometer to determine the total copper concentration of the water sample to be detected.
5. Test results
The total copper concentration in water samples of different turbidity chromaticities was determined using the method of this example and the national standard method, and the test results are shown in table 4.
TABLE 4
As can be seen from Table 4, the measurement results of two different water samples which do not pass turbidity chromaticity correction have larger difference with the national standard measurement results, and the relative errors are respectively 25.09% and 118.8%; after turbidity chromaticity correction, the total copper concentration in the measured water sample is close to the national standard measurement result, and the relative errors are-4.03% and 1.52% respectively. The method for correcting the total copper turbidity chromaticity provided by the invention is effective in the measurement of an actual water sample and has high accuracy.
Example 3
The embodiment provides a total phosphorus turbidity chromaticity correction method for automatic water quality monitoring, which comprises the following steps:
1. preparation of the solution
The phosphorus standard solution is prepared by the following steps:
1) 0.2197 +/-0.0001 g of potassium dihydrogen phosphate is accurately weighed, dried at 110 ℃ for 2h and cooled in a dryer, dissolved by adding a small amount of ultrapure water, transferred to a 100mL volumetric flask, added with about 800mL of ultrapure water, added with 5.0mL of (1+1) sulfuric acid, and continuously diluted with ultrapure water to the marked line, thus obtaining the standard stock solution of phosphorus with the concentration of 50 mg/L.
2) Accurately transferring 10.0mL of the standard stock solution of phosphorus with the concentration of 50mg/L into a volumetric flask with the volume of 250mL, using ultrapure water to fix the volume to a scale, and shaking up to obtain the standard use solution of phosphorus with the concentration of 2 mg/L.
3) 1mL, 2.0mL, 6.0mL, 10.0mL, 20.0mL and 30.0mL of phosphorus standard use solution with the concentration of 2mg/L are respectively and accurately transferred and placed in a 50mL volumetric flask, the volume is fixed to a marked line by ultrapure water, and the phosphorus standard solution with the concentration of 0.04mg/L, 0.08mg/L, 0.24mg/L, 0.40mg/L, 0.80mg/L and 1.20mg/L is respectively obtained after shaking up.
The preparation method of the potassium persulfate solution comprises the following steps:
5.0g of potassium persulfate powder was weighed into a 100mL beaker, dissolved completely in a small amount of ultrapure water, transferred to a 100mL volumetric flask, and diluted with ultrapure water to the marked line to obtain 50g/L of potassium persulfate solution.
The ascorbic acid is prepared by the following steps:
weighing 10.0g ascorbic acid into a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring into a 100mL volumetric flask, and diluting with ultrapure water to a marked line to obtain 100g/L ascorbic acid solution.
The molybdate solution is prepared by the following steps:
weighing 13.0g of ammonium molybdate and 0.35g of antimony potassium tartrate, dissolving the ammonium molybdate and the antimony potassium tartrate in 100mL of ultrapure water, slowly adding the ammonium molybdate solution and the antimony potassium tartrate solution into 300mL (1+1) of sulfuric acid under continuous stirring, then adding the antimony potassium tartrate solution, uniformly mixing, transferring the mixture into a brown reagent bottle, and storing the mixture in a cold place for 2 months.
The turbidity chroma compensation liquid preparation steps are as follows:
2 volumes of (1+1) sulfuric acid and 1 volume of 100g/L ascorbic acid were removed and mixed well and prepared for use on the same day.
2. Drawing a working curve
Respectively putting 2.5mL of phosphorus standard solution with the concentrations of 0.00mg/L, 0.04mg/L, 0.08mg/L, 0.24mg/L, 0.40mg/L, 0.80mg/L and 1.20mg/L into a 10mL digestion tube, adding 0.4mL of 50g/L potassium persulfate, sealing, heating at 120 ℃ for 30min, taking out, cooling to room temperature by tap water, adding 2.1mL of ultrapure water, adding 0.1mL of 100g/L ascorbic acid, shaking for 30s, adding 0.2mL of molybdate solution, standing for 15min, and determining the absorbance A at 700nm by using the pure water as a reference. And drawing a standard curve by taking the concentration of phosphorus as an abscissa and the corresponding absorbance as an ordinate. The equation is that y is 0.3264x +0.0015, the linear range of total phosphorus is 0-1.2 mg/L, and the correlation coefficient r2＝0.9998。
In this example, the standard curve of the total phosphorus concentration of the standard solution with absorbance is shown in table 5 and fig. 3.
TABLE 5 Standard Curve of Total phosphorus concentration versus Absorbance of Standard solutions
3. Determination of water sample to be measured
Taking 2.5mL of a water sample to be detected into a 10mL digestion tube, adding 0.4mL of 50g/L potassium persulfate, sealing, heating at 120 ℃ for 30min, taking out, cooling to room temperature, adding 2.1mL of ultrapure water, adding 0.1mL of 100g/L ascorbic acid, shaking for 30s, taking pure water as a reference at a wavelength of 700nm, determining the absorbance A1 of the water sample before color development, finally adding 0.2mL of molybdate solution, shaking uniformly, standing for 15min, taking pure water as a reference at a wavelength of 700nm, determining the absorbance A2 of the water sample after color development, obtaining the absorbance A of the water sample to be detected through correction, and calculating the total phosphorus concentration of the water sample to be detected according to a standard curve.
And (3) correction of the absorbance value: the absorbance a1 was corrected based on the volume V1 at the time of measurement of a1 and the volume V2 at the time of measurement of a2, i.e., a1 ═ a1 (V1/V2), and the difference between a2 and a1 ', i.e., Δ a ═ a2-a 1', was used as the absorbance a of the sample after correction.
4. Testing the total phosphorus concentration of the water sample to be tested by the national standard method
Taking 2.5mL of water sample to be detected, adding 0.4mL of 50g/L potassium persulfate into a 10mL digestion tube, sealing, heating at 120 ℃ for 30min, taking out, cooling to room temperature, adding 2.1mL of ultrapure water, adding 0.1mL of 100g/L ascorbic acid, shaking for 30s, adding 0.2mL of molybdate solution, standing for 15min, and determining absorbance A1 at 700nm by taking pure water as a reference; another set of parallel measurements was made, but a mixed solution of two volumes (1+1) of sulfuric acid and one volume of ascorbic acid of 50g/L was used as a colorimetric-turbidity colorimetric compensation solution instead of the ascorbic acid and molybdate solution, and the absorbance was measured as A0. And (4) calculating A-A1-A0, and calculating the total phosphorus concentration of the water sample to be detected according to the standard curve.
5. Test results
The total phosphorus concentration in water samples of different turbidity chromaticities was determined using the method of this example and the national standard method, and the test results are shown in table 6.
TABLE 6
As can be seen from Table 6, the measurement results of two different water samples, which did not pass the turbidity chromaticity correction, differed greatly from the national standard measurement values, with relative errors of 135.93% and 50.36%, respectively; after turbidity chromaticity correction, the total phosphorus concentration of the measured water sample is close to the value measured by the national standard method, and the relative errors are-8.47 percent and-3.41 percent respectively. The method for correcting the total phosphorus turbidity chromaticity provided by the invention is effective in the measurement of an actual water sample and has high accuracy.
Example 4
The embodiment provides an ammonia nitrogen turbidity chromaticity correction method for automatic water quality monitoring, which comprises the following steps:
1. preparation of the solution
The steps for preparing the ammonia nitrogen standard solution are as follows:
1) 3.8190g of ammonium chloride (superior pure, 100-. The solution was stable for one month.
2) Accurately transferring 10.0mL of 1000mg/L ammonia nitrogen standard stock solution into a 100mL volumetric flask, performing constant volume to scale with ultrapure water, and shaking up to obtain 100mg/L ammonia nitrogen standard intermediate solution.
3) Accurately transferring 1.0mL of 100mg/L ammonia nitrogen standard intermediate solution, placing in a 100mL volumetric flask, performing constant volume to the marked line by using ultrapure water, and shaking up to obtain the ammonia nitrogen standard use solution with the concentration of 1 mg/L.
The color developing agent (salicylic acid-potassium sodium tartrate solution) is prepared by the following steps:
25.0g of salicylic acid [ C ] was weighed6H4(OH)COOH]Adding 80mL of 2mol/L sodium hydroxide solution into a 100mL beaker, stirring to completely dissolve the powder (5 mL of sodium hydroxide can be added when the powder is not completely dissolved), and adjusting the pH value to 6-6.5 by using dilute sulfuric acid; 25.0g of sodium potassium tartrate was weighed into a 100mL beaker, stirred with a small amount of ultrapure water until completely dissolved, combined with the above solution and transferred to a 1000mL volumetric flask, diluted with ultrapure water to the marked line and stored in a brown glass bottle. The solution was stable for one month.
The preparation method of the sodium nitrosoferricyanide solution comprises the following steps:
weighing 1.0g of sodium nitroferricyanide in a 100mL beaker, adding a small amount of ultrapure water to dissolve completely, transferring the solution into a 100mL volumetric flask, and diluting the solution with ultrapure water to a marked line to obtain 10g/L of sodium nitroferricyanide solution.
The preparation method of the sodium hypochlorite solution comprises the following steps:
taking a calibrated sodium hypochlorite solution, diluting the sodium hypochlorite solution into a sodium hypochlorite use solution containing 3.5g/L of available chlorine and 0.75mol/L (calculated by NaOH) of free alkali by using ultrapure water and 2mol/L sodium hydroxide solution, and storing the sodium hypochlorite use solution in a brown bottle, wherein the solution can be stable for one month.
2. Drawing a working curve
Accurately transferring 0.0mL, 1.0mL, 2.0mL, 4.0mL, 6.0mL and 8.0mL of ammonia nitrogen standard use solution with the concentration of 1mg/L respectively, placing the solution in a 10mL digestion tube, fixing the volume to 8mL by using ultrapure water, shaking up to obtain ammonia nitrogen standard solutions with the concentrations of 0.000mg/L, 0.125mg/L, 0.250mg/L, 0.500mg/L, 0.750mg/L and 1.000mg/L respectively, adding 1.0mL of a color developing agent (a salicylic acid-potassium sodium tartrate solution), adding 0.1mL of a sodium nitrosoferricyanide solution, mixing uniformly, adding 0.1mL of a sodium hypochlorite use solution, adding 0.8mL of ultrapure water, shaking up to fix the volume, developing for 60min, and then determining the absorbance A by using pure water as a reference at 697 nm. And drawing a standard curve by taking the concentration of ammonia nitrogen as an abscissa and the corresponding absorbance as an ordinate. The equation is that y is 1.0883x +0.0158, the linear range of ammonia nitrogen is 0-1.0 mg/L, and the correlation coefficient r2Is 0.9990.
In this example, the standard curve of ammonia nitrogen concentration versus absorbance of the standard solution is shown in table 7 and fig. 4.
TABLE 7 Standard Curve of Ammonia Nitrogen concentration and Absorbance of Standard solution
3. Determination of water sample to be measured
Putting 8.0mL of water sample to be detected into a 10mL digestion tube, adding 1.0mL of salicylic acid-potassium sodium tartrate solution, uniformly mixing, taking pure water as a reference at a wavelength of 697nm, and determining the absorbance A1 of the water sample to be detected before color development. And then adding 0.1mL of sodium nitrosoferricyanide solution, shaking up, then adding 0.1mL of sodium hypochlorite solution, then adding 0.8mL of ultrapure water for constant volume, shaking up, developing for 60min, then taking pure water as a reference at 697nm, determining the absorbance A2 of the developed water sample, obtaining the corrected absorbance A of the water sample to be detected through correction, and calculating the ammonia nitrogen concentration of the water sample to be detected according to a standard curve.
And (3) correction of the absorbance value: the absorbance a1 was corrected based on the volume V1 at the time of measurement of a1 and the volume V2 at the time of measurement of a2, i.e., a1 ═ a1 (V1/V2), and the difference between a2 and a1 ', i.e., Δ a ═ a2-a 1', was used as the absorbance a of the sample after correction.
4. Testing the ammonia nitrogen concentration of the water sample to be tested by the national standard method
Flocculating and precipitating a water sample to be detected: adding 1mL of zinc sulfate solution into 100mL of water sample to be detected, then adding 0.1-0.2 mL of 250g/L of sodium hydroxide solution, adjusting the pH to be about 10.5, uniformly mixing, standing for precipitating for 15min, and pouring out supernate for analysis.
Putting 8.0mL of water sample to be detected after flocculation precipitation into a 10mL digestion tube, adding 1.0mL of salicylic acid-potassium sodium tartrate solution, then adding 0.1mL of sodium nitroferricyanide solution, mixing uniformly, then adding 0.1mL of sodium hypochlorite solution, then adding 0.8mL of ultrapure water to constant volume, shaking uniformly, and developing for 60 min. And (3) taking pure water as a reference at 697nm, determining the absorbance A of the water sample to be detected, and calculating the ammonia nitrogen concentration of the water sample to be detected according to a standard curve.
5. Test results
The ammonia nitrogen concentrations in water samples with different turbidity chromaticities were measured by the method of this example and the national standard method, and the test results are shown in table 8.
TABLE 8
As can be seen from Table 8, the measurement results of two different water samples which are not corrected by chromaticity have larger difference with the concentration measured by the national standard method, and the relative errors are 39.81 percent and 71.76 percent respectively; after the chromaticity correction, the measured ammonia nitrogen concentration of the water sample is close to the concentration measured by the national standard method, and the relative errors are respectively 3.52 percent and-5.54 percent. The ammonia nitrogen chromaticity correction method provided by the invention is effective in the measurement of the actual water sample and has high accuracy.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (2)
1. A turbidity chromaticity correction method for an automatic water quality monitor is characterized by comprising the following steps:
(1) drawing a standard curve: preparing a series of standard solutions with different concentrations, testing the absorbance of the solutions in a spectrophotometer/automatic monitoring equipment after digestion, and establishing a standard curve to obtain a linear relation equation of the concentration of the standard solution and the absorbance of the standard solution;
(2) and (3) determining a sample: taking pure water as reference, determining the absorbance A1 of the water sample to be detected before color development, adding a color developing agent, determining the absorbance A2 of the water sample to be detected after color development, and recording the volume V1 of the water sample to be detected before color development and the volume V2 of the water sample to be detected after color development;
(3) and (3) correcting the absorbance value: correcting the absorbance A1 before the color development of the water sample to be detected according to the volume V1 when A1 is measured and the volume V2 when A2 is measured, wherein the correction formula is as follows: a 1' ═ a1 (V1/V2);
(4) and (3) calculating the concentration: and (3) substituting the absorbance A of the obtained water sample to be detected into the standard curve in the step (1) to calculate the concentration of the water sample to be detected, wherein the difference value of the absorbance A2 of the water sample to be detected after color development and the absorbance A1' of the water sample to be detected before color development after correction is the absorbance A of the water sample to be detected.
2. The turbidity chromaticity correction method for the water quality automatic monitor according to claim 1, characterized in that the standard working curve obtained in step (1) is as follows: k x + b
Wherein y is the absorbance of the standard solution, x is the concentration of the standard solution, k is the slope coefficient of the reticle, and b is the intercept coefficient of the reticle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111083329.5A CN113884450A (en) | 2021-09-15 | 2021-09-15 | Turbidity chromaticity correction method for automatic water quality monitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111083329.5A CN113884450A (en) | 2021-09-15 | 2021-09-15 | Turbidity chromaticity correction method for automatic water quality monitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113884450A true CN113884450A (en) | 2022-01-04 |
Family
ID=79009613
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111083329.5A Pending CN113884450A (en) | 2021-09-15 | 2021-09-15 | Turbidity chromaticity correction method for automatic water quality monitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113884450A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116559393A (en) * | 2022-09-30 | 2023-08-08 | 五邑大学 | Method for detecting ammonia nitrogen content by utilizing nitrifying biological reaction |
| WO2024046369A1 (en) * | 2022-08-31 | 2024-03-07 | 上海博取仪器有限公司 | Anti-interference water quality analysis instrument test method |
| CN117805046A (en) * | 2024-02-28 | 2024-04-02 | 三亚海慧海洋科技有限公司 | Method and device for detecting chemical oxygen demand based on turbidity compensation |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005214724A (en) * | 2004-01-28 | 2005-08-11 | Nippon Denshoku Kogyo Kk | Chromaticity measuring method |
| CN103743682A (en) * | 2013-12-13 | 2014-04-23 | 金川集团股份有限公司 | Differential spectrophotometry measuring method |
| CN104020118A (en) * | 2014-05-28 | 2014-09-03 | 安徽工程大学 | Method for continuously determining trace elements in tea leaves |
| CN108956490A (en) * | 2018-06-05 | 2018-12-07 | 山东省科学院海洋仪器仪表研究所 | A kind of determining amount method for total nitrogen total phosphorus analyzer |
| CN109187388A (en) * | 2018-09-05 | 2019-01-11 | 安徽润安信科检测科技有限公司 | A kind of colorimetry-turbidity compensation measuring method of Liquor-making industry ammonia nitrogen in waste water |
| CN109557245A (en) * | 2018-12-11 | 2019-04-02 | 贵州航天精工制造有限公司 | Standard reagent and its preparation method applied to electroplating wastewater processing on-line monitoring system |
| CN109580480A (en) * | 2017-09-28 | 2019-04-05 | 株式会社岛津制作所 | Total phosphorus determination device |
| CN109827955A (en) * | 2018-12-21 | 2019-05-31 | 鞍钢实业微细铝粉有限公司 | A kind of nickel aluminium composite powder nickel content detection method |
| CN112611725A (en) * | 2020-11-25 | 2021-04-06 | 江苏启辰检测科技有限公司 | Method for detecting ammonia nitrogen content in printing and dyeing wastewater |
-
2021
- 2021-09-15 CN CN202111083329.5A patent/CN113884450A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005214724A (en) * | 2004-01-28 | 2005-08-11 | Nippon Denshoku Kogyo Kk | Chromaticity measuring method |
| CN103743682A (en) * | 2013-12-13 | 2014-04-23 | 金川集团股份有限公司 | Differential spectrophotometry measuring method |
| CN104020118A (en) * | 2014-05-28 | 2014-09-03 | 安徽工程大学 | Method for continuously determining trace elements in tea leaves |
| CN109580480A (en) * | 2017-09-28 | 2019-04-05 | 株式会社岛津制作所 | Total phosphorus determination device |
| CN108956490A (en) * | 2018-06-05 | 2018-12-07 | 山东省科学院海洋仪器仪表研究所 | A kind of determining amount method for total nitrogen total phosphorus analyzer |
| CN109187388A (en) * | 2018-09-05 | 2019-01-11 | 安徽润安信科检测科技有限公司 | A kind of colorimetry-turbidity compensation measuring method of Liquor-making industry ammonia nitrogen in waste water |
| CN109557245A (en) * | 2018-12-11 | 2019-04-02 | 贵州航天精工制造有限公司 | Standard reagent and its preparation method applied to electroplating wastewater processing on-line monitoring system |
| CN109827955A (en) * | 2018-12-21 | 2019-05-31 | 鞍钢实业微细铝粉有限公司 | A kind of nickel aluminium composite powder nickel content detection method |
| CN112611725A (en) * | 2020-11-25 | 2021-04-06 | 江苏启辰检测科技有限公司 | Method for detecting ammonia nitrogen content in printing and dyeing wastewater |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024046369A1 (en) * | 2022-08-31 | 2024-03-07 | 上海博取仪器有限公司 | Anti-interference water quality analysis instrument test method |
| CN116559393A (en) * | 2022-09-30 | 2023-08-08 | 五邑大学 | Method for detecting ammonia nitrogen content by utilizing nitrifying biological reaction |
| CN116559393B (en) * | 2022-09-30 | 2024-02-09 | 五邑大学 | Method for detecting ammonia nitrogen content by utilizing nitrifying biological reaction |
| CN117805046A (en) * | 2024-02-28 | 2024-04-02 | 三亚海慧海洋科技有限公司 | Method and device for detecting chemical oxygen demand based on turbidity compensation |
| CN117805046B (en) * | 2024-02-28 | 2024-06-04 | 三亚海慧海洋科技有限公司 | Method and device for detecting chemical oxygen demand based on turbidity compensation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113884450A (en) | Turbidity chromaticity correction method for automatic water quality monitor | |
| CN107356539A (en) | A kind of method of nitrogen nutrition salinity in quick detection seawater | |
| CN101713739B (en) | Reagent and method for determining chemical oxygen demand of high-chloride wastewater | |
| CN110987918A (en) | Detection reagent and rapid detection method for total nitrogen in water | |
| US20210270794A1 (en) | Method of determining chemical oxygen demand (cod) for high chloride samples | |
| CN116840219A (en) | Method for detecting total nitrogen concentration of water quality | |
| CN115950843A (en) | Improved iodine oxidation-dimethylglyoxime photometric method for detecting nickel content in steel | |
| CN109682808A (en) | A kind of improved faintly acid water body Central Asia nitrate nitrogen content measuring method | |
| CN112504980B (en) | Detection method of imidazoline corrosion inhibitor and application thereof | |
| CN115561186A (en) | Method for determining glucose in lithium-ion electrolytic copper foil electroplating solution | |
| CN112255225B (en) | Method for testing COD (chemical oxygen demand) of organic matters in waste hydrochloric acid containing iron | |
| CN109827916B (en) | Water quality nitrate detection method based on zinc-cadmium reduction salt-free effect | |
| CN113655012A (en) | high-COD (chemical oxygen demand) wastewater total nitrogen testing method | |
| CN111257251A (en) | Method for measuring potassium content | |
| CN112345479A (en) | Method for measuring chloride ion content in cobaltosic oxide by using double-beam turbidimetry | |
| CN111912800A (en) | Method for detecting low-concentration ammonia nitrogen in drinking water | |
| CN116285967B (en) | Silicon-doped carbon quantum dot, preparation method and application thereof in detection of mercapto compound content in urine | |
| CN113916815B (en) | Method for measuring content of ammonia nitrogen in seawater by using Nashin's reagent spectrophotometry | |
| WO2024007482A1 (en) | Solid reagent for detection of ammonia nitrogen and detection method therefor | |
| CN112504982B (en) | Water quality total nitrogen detection method | |
| CN112161970A (en) | Method for determining total phosphorus content in water | |
| CN114371165B (en) | Method for detecting silicon dioxide content in high-chroma and reductive wastewater | |
| Qiao et al. | Spectrophotometric studies and applications for the determination of Ni2+ in zinc–nickel alloy electrolyte | |
| CN112362651B (en) | Thiocyanate determination method with stable color development | |
| CN112305150A (en) | Method for detecting nickel in nickel plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |