CN117929363A - Silicate detection reagent, detection kit and detection method - Google Patents
Silicate detection reagent, detection kit and detection method Download PDFInfo
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- CN117929363A CN117929363A CN202311742160.9A CN202311742160A CN117929363A CN 117929363 A CN117929363 A CN 117929363A CN 202311742160 A CN202311742160 A CN 202311742160A CN 117929363 A CN117929363 A CN 117929363A
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 110
- 238000001514 detection method Methods 0.000 title claims abstract description 56
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000000873 masking effect Effects 0.000 claims abstract description 17
- 239000012445 acidic reagent Substances 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 26
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 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 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 150000008107 benzenesulfonic acids Chemical class 0.000 claims description 12
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 10
- 229960005070 ascorbic acid Drugs 0.000 claims description 10
- 235000010323 ascorbic acid Nutrition 0.000 claims description 10
- 239000011668 ascorbic acid Substances 0.000 claims description 10
- 239000011609 ammonium molybdate Substances 0.000 claims description 9
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 239000011550 stock solution Substances 0.000 claims description 7
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 6
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 3
- JUSXLWAFYVKNLT-UHFFFAOYSA-N 2-bromobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1Br JUSXLWAFYVKNLT-UHFFFAOYSA-N 0.000 claims description 3
- MNURPFVONZPVLA-UHFFFAOYSA-N 2-chlorobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1Cl MNURPFVONZPVLA-UHFFFAOYSA-N 0.000 claims description 3
- QDWTXRWOKORYQH-UHFFFAOYSA-N 3-bromobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC(Br)=C1 QDWTXRWOKORYQH-UHFFFAOYSA-N 0.000 claims description 3
- IQOJIHIRSVQTJJ-UHFFFAOYSA-N 3-chlorobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC(Cl)=C1 IQOJIHIRSVQTJJ-UHFFFAOYSA-N 0.000 claims description 3
- PXACTUVBBMDKRW-UHFFFAOYSA-N 4-bromobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(Br)C=C1 PXACTUVBBMDKRW-UHFFFAOYSA-N 0.000 claims description 3
- RJWBTWIBUIGANW-UHFFFAOYSA-N 4-chlorobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(Cl)C=C1 RJWBTWIBUIGANW-UHFFFAOYSA-N 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052794 bromium Inorganic materials 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 239000011790 ferrous sulphate Substances 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 3
- 239000011630 iodine Substances 0.000 claims description 3
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 235000007686 potassium Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- 235000015393 sodium molybdate Nutrition 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 125000001424 substituent group Chemical group 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical class OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 3
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid group Chemical group S(N)(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000011161 development Methods 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000011574 phosphorus Substances 0.000 description 8
- 229910052698 phosphorus Inorganic materials 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- KQROHCSYOGBQGJ-UHFFFAOYSA-N 5-Hydroxytryptophol Chemical compound C1=C(O)C=C2C(CCO)=CNC2=C1 KQROHCSYOGBQGJ-UHFFFAOYSA-N 0.000 description 6
- 239000010865 sewage Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000011964 heteropoly acid Substances 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 235000013405 beer Nutrition 0.000 description 2
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000008235 industrial water Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 2
- 235000019799 monosodium phosphate Nutrition 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000149 chemical water pollutant Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a silicate detection reagent, a detection kit and a detection method, wherein the detection reagent comprises a reagent 1, a reagent 2 and a reagent 3; the reagent 1 comprises a strong acid reagent and a weighting agent, wherein the mass ratio of the strong acid reagent to the weighting agent is (1-10): 2-10; the reagent 2 comprises molybdate and water, wherein the mass volume ratio (g: mL) of the molybdate to the water is (1-50): 1-50; the reagent 3 comprises masking agent, reducing agent and water, wherein the mass volume ratio (g: g: mL) of the masking agent to the reducing agent to the water is (2-30): 10-50): 1-100. The detection reagent has no special environmental requirement, no special three-waste pollution, low cost, simple detection steps, no interference, more accurate measurement, short color development time and strong mobility.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a silicate radical detection reagent, a silicate radical detection kit and a silicate radical detection method.
Background
Almost all industrial production processes need water, and the quality of water has different influences on the production process or products. The silicon content in water is also a normal measurement parameter of water quality, and too high content not only increases the generation amount of scale but also increases the hardness of the scale. After the silicon dioxide in the circulating cooling water exceeds the limit concentration, the pipeline is easy to be blocked, and even serious accidents are caused. In order to prevent accidents, the silicon content in industrial water needs to be detected in real time, and when the silicon content is too high, the industrial water needs to be subjected to silicon removal treatment.
There are also many methods for detecting silicate groups, such as gravimetric, titrimetric and spectrophotometric methods. The weight method generally comprises a secondary hydrochloric acid evaporation dehydration method, a primary hydrochloric acid evaporation dehydration method, a chlorination method, a polyethylene oxide condensation weight method and an animal gel polymerization weight method. Titration is commonly used for measuring silica in cement, metallurgy, novel inorganic materials, glass products and raw materials thereof. Spectrophotometry is applied to a large number of water quality detection industries, silicon and phosphate react with molybdate in an acidic environment to generate yellow silicon-molybdenum heteropolyacid complexes and group heteropolyacid complexes, and the addition of citric acid and the like can destroy the phosphorus-containing complexes, and only yellow silicon-containing compounds are left for quantitative determination. When the silicon content is high, the left yellow color is darker, the color depth is proportional to the concentration of effective silicon, and the method accords with the lambert beer law in a certain range, so that the colorimetric method can be used for measurement. However, the detection method requires specific equipment, has high cost, complex operation, high professional requirements, difficult emergency and the like, and limits the application of the detection method in rapid detection. In order to complement the short plates of the detection, silicate detection kits which are rapid, accurate, convenient to carry, simple to operate and quick have been developed in recent years.
The existing silicate detection kit is based on the reaction principle of silicon molybdenum yellow or silicon molybdenum blue. In an acidic solution, silicic acid and ammonium molybdate form yellow silicomolybdenum heteropolyacid (silicomolybdenum Huang Fa), phosphorus is masked by oxalic acid, and the silicomolybdenum heteropolyacid is reduced into a silicomolybdenum blue complex (silicomolybdenum blue method) by using ascorbic acid, wherein the color depth is in direct proportion to the concentration of effective silicon, accords with the lambert beer law in a certain range, and can be measured by a colorimetric method. However, in actual practice, these kits are found to be generally high in false positive ratio, and cannot eliminate interference of elements such as arsenic, phosphorus and the like. Thus, improving the measurement sensitivity of the kit and eliminating interference from other elements is a critical problem that needs to be solved at present. In addition, the silicate detection kit or silicate detection test paper sold in the market at present needs multiple steps to operate, is not suitable for field operation, has short reagent storage period and is not easy to store for a long time. Thus, there is an urgent need to improve the existing methods for determining silicate.
The Chinese patent with publication number of CN115931757A provides a reagent combination for measuring silicate, a preparation method thereof and a method for measuring silicate, and silicate can be measured by using non-dangerous raw materials, so that the reagent cost for measuring silicate is reduced and the safety of experimental personnel is improved. However, the disadvantage is that the interference of elements such as arsenic and phosphorus cannot be eliminated.
The Chinese patent with publication number CN114371165A shields the interference of high-interference waste water such as domestic sewage, landfill leachate or diluted sewage with too high concentration, which has higher chromaticity and reducing substances, by arranging an acidification step, an oxidation step and a color development step, but the pretreatment steps of the sewage are all pretreatment steps of the sewage, and the molybdenum blue color development method is not improved and the interference of elements such as arsenic, phosphorus and the like cannot be eliminated.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provides a silicate radical detection reagent, a silicate radical detection kit and a silicate radical detection method.
In one aspect, the invention provides a silicate detection reagent, which comprises a reagent 1, a reagent 2 and a reagent 3;
The reagent 1 comprises a strong acid reagent and a weighting agent, wherein the mass ratio of the strong acid reagent to the weighting agent is (1-10): 2-10;
The reagent 2 comprises molybdate and water, wherein the mass volume ratio (g: mL) of the molybdate to the water is (1-50): 1-50;
The reagent 3 comprises masking agent, reducing agent and water, wherein the mass volume ratio (g: g: mL) of the masking agent to the reducing agent to the water is (2-30): 10-50): 1-100.
Further, the strong acid reagent is selected from one or more of sulfamic acid, citric acid, glycolic acid, benzenesulfonic acid, substituted benzenesulfonic acid and trichloroacetic acid;
The molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
the masking agent comprises one or more of citric acid, oxalic acid, tartaric acid and EDTA;
The reducing agent comprises one or more of ferrous sulfate, ascorbic acid and stannic chloride;
The weighting agent includes one or more of sodium chloride, sodium sulfate, potassium sulfate.
Further, the substituent of the substituted benzenesulfonic acid is selected from C1-C4 alkyl, chlorine, bromine or iodine;
Preferably, the substituted benzene sulfonic acid comprises o-C1-C4 alkyl benzene sulfonic acid, m-C1-C4 alkyl benzene sulfonic acid, p-C1-C4 alkyl benzene sulfonic acid, o-chloro benzene sulfonic acid, m-chloro benzene sulfonic acid, p-chloro benzene sulfonic acid, o-bromo benzene sulfonic acid, m-bromo benzene sulfonic acid and p-bromo benzene sulfonic acid;
Preferably, the substituted benzenesulfonic acid is selected from p-toluenesulfonic acid.
Further, the strongly acidic reagent is selected from sulfamic acid;
The molybdate is selected from ammonium molybdate;
the masking agent is selected from oxalic acid;
The reducing agent is selected from ascorbic acid;
the weighting agent is selected from sodium chloride.
In another aspect, the invention provides a silicate radical detection kit, which comprises the detection reagent.
Further, the kit also comprises a standard color chart.
In another aspect, the present invention provides a method for preparing the above-mentioned detection kit, comprising the steps of:
preparation of reagent 1: fully grinding the strong acid reagent and the weighting agent according to the proportion, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by introducing inert gas;
preparation of reagent 2: dissolving molybdate in water according to a proportion;
Preparation of reagent 3: according to the proportion, the masking agent and the reducing agent are dissolved in water.
Further, the reagent 1 is divided into 0.1-0.5 g for each tube.
Further, the preparation method further comprises the preparation of a standard color chart: preparing silicate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L by adopting silicon dioxide stock solution, taking 1-5 ml of each silicate standard solution, respectively adding the silicate standard solutions into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, and developing for 1-5 min to obtain the standard colorimetric card.
The invention also provides a detection method of silicate radicals, which adopts the detection kit to detect, and comprises the following steps: adding 1-5 mL of water sample to be detected into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, developing for 1-5 min, comparing with a standard colorimetric card, and determining the concentration of silicate in the water sample to be detected.
The detection kit is stored in a shade and dry place, and the storage temperature is preferably lower than 26 ℃. If the temperature is higher than 25 ℃, the unused test paper bag is put into a fresh-keeping layer in a refrigerator for preservation, and is put into a package which is light-proof and moisture-proof for preservation. The effective service life of the detection kit is about one year.
The beneficial effects of the invention are as follows:
1. The silicate radical detection method is based on a silico-molybdenum blue method, and is a rapid and flexible silicate radical rapid detection method which does not need instruments and equipment and has low production and use costs. The kit has the advantages of no special environmental requirement, no special three-waste pollution, low cost, simple detection steps, no interference, more accurate measurement, short color development time and strong mobility. Compared with the traditional method or other measurement forms, the invention is more convenient to use and does not need special technicians to measure. The reagents used in the invention are all common chemical reagents, safe and reliable and low in cost. The method has wide application range, and can be used for measuring the silicate content of the water bodies such as chemical sewage, surface water, urban sewage recycling-landscape environmental water, urban miscellaneous water and the like, in particular to the monitoring of environment-friendly silicate.
2. The silicate detection kit reduces the dosage of acid by controlling the acidity, so as to reduce the interference of phosphorus, has strong anti-interference capability when being used for detecting silicate in a water sample, has short detection time, can be completed in 5 minutes, is simple to operate, has small volume and can be carried about.
Drawings
FIG. 1 is a standard color chart of a detection kit of the present invention;
FIG. 2 shows the color development results of example 1;
FIG. 3 shows the color development results of example 2;
FIG. 4 shows the color development results of example 3;
FIG. 5 shows the color development results of example 4.
Detailed Description
For a clearer understanding of the present invention, the present invention will now be further described with reference to the following examples and drawings. The examples are for illustration only and are not intended to limit the invention in any way. In the examples, each of the starting reagent materials is commercially available, and the experimental methods without specifying the specific conditions are conventional methods and conventional conditions well known in the art, or according to the conditions recommended by the instrument manufacturer.
The embodiment provides a silicate radical detection kit, which comprises a reagent 1, a reagent 2, a reagent 3 and a standard colorimetric card, wherein the reagent 1 comprises a strong acid reagent and a weighting agent, and the mass ratio of the strong acid reagent to the weighting agent is (1-10) (2-10); the reagent 2 comprises molybdate and water, wherein the mass volume ratio (g: mL) of the molybdate to the water is (1-50): 1-50; the reagent 3 comprises masking agent, reducing agent and water, wherein the mass volume ratio (g: g: mL) of the masking agent to the reducing agent to the water is (2-30): (10-50): (1-100). The preparation method comprises the following steps:
Preparation of reagent 1: fully grinding the strong acid reagent and the weighting agent according to the proportion, enabling the ground mixed components to pass through an 80-target standard sieve, sub-packaging, and vacuumizing or sealing by introducing inert gas; preferably, the reagent 1 is divided into 0.1 to 0.5g per tube;
preparation of reagent 2: dissolving molybdate in water according to a proportion;
Preparation of reagent 3: according to the proportion, the masking agent and the reducing agent are dissolved in water.
Standard colorimetric card preparation: preparing silicate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L by adopting silicon dioxide stock solution, taking 1-5 ml of each silicate standard solution, respectively adding the silicate standard solutions into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, and developing for 1-5 min to obtain the standard colorimetric card. If silicate exists in water, the blue-green color is displayed, the color depth is related to the concentration of silicate in water, and the silicate is compared with a standard color chart to determine the concentration of silicate in the water sample to be detected.
Wherein the strong acid reagent is selected from one or more of sulfamic acid, citric acid, glycolic acid, benzenesulfonic acid, substituted benzenesulfonic acid and trichloroacetic acid; preferably, the substituent of the substituted benzenesulfonic acid is selected from C1-C4 alkyl, chlorine, bromine or iodine; preferably, the substituted benzene sulfonic acid comprises o-C1-C4 alkyl benzene sulfonic acid, m-C1-C4 alkyl benzene sulfonic acid, p-C1-C4 alkyl benzene sulfonic acid, o-chloro benzene sulfonic acid, m-chloro benzene sulfonic acid, p-chloro benzene sulfonic acid, o-bromo benzene sulfonic acid, m-bromo benzene sulfonic acid and p-bromo benzene sulfonic acid; preferably, the substituted benzenesulfonic acid is selected from p-toluenesulfonic acid.
The molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate.
The masking agent comprises one or more of citric acid, oxalic acid, tartaric acid, and EDTA.
The reducing agent comprises one or more of ferrous sulfate, ascorbic acid and stannic chloride.
The weighting agent comprises one or more of sodium chloride, sodium sulfate and potassium sulfate, and the addition of the weighting agent facilitates the weighing of the powder.
Example 1
The embodiment provides a silicate radical detection kit, which comprises a reagent 1, a reagent 2, a reagent 3 and a standard colorimetric card.
Preparation of reagent 1: 2g of sulfamic acid and 8g of sodium chloride are added into a mortar, fully ground until all raw materials can pass through an 80-target standard sieve, and then sub-packaged into 0.2g of each tube, and vacuumized or sealed by inert gas.
Preparation of reagent 2: ammonium molybdate 0.5g was dissolved in 5mL of water.
Preparation of reagent 3: oxalic acid 1g and ascorbic acid 4g were dissolved in 10mL of water.
Preparing a silicate standard solution with the concentration of 0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L by adopting a silicon dioxide stock solution, taking 1-5 ml of each silicate standard solution, respectively adding the silicate standard solution into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, and developing for 1-5 min to obtain the standard colorimetric card. If silicate exists in water, bluish green color is displayed, and the shade of the color is related to the concentration of silicate in water.
The prepared standard color chart is shown in figure 1, and the color development result is shown in figure 2.
Example 2
The embodiment provides a detection kit, which comprises a reagent 1, a reagent 2 and a reagent 3.
Preparation of reagent 1: 2g of sulfamic acid and 8g of sodium chloride are added into a mortar, fully ground until all raw materials can pass through an 80-target standard sieve, and then sub-packaged into 0.2g of each tube, and vacuumized or sealed by inert gas.
Preparation of reagent 2: ammonium molybdate 0.5g was dissolved in 5mL of water.
Preparation of reagent 3: 4g of ascorbic acid was dissolved in 10mL of water.
Preparing phosphate standard solutions with the concentration of 0mg/L, 0.5mg/L, 1mg/L, 2mg/L, 4mg/L, 8mg/L, 15mg/L, 30mg/L, 60mg/L, 120mg/L and 250mg/L by adopting sodium dihydrogen phosphate stock solution, taking 1-5 ml of each phosphate standard solution, respectively adding the phosphate standard solutions into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, and developing for 1-5 min, wherein the result is shown in figure 3. The reagent kit can not eliminate the interference of elements such as phosphorus without adding a masking agent.
Example 3
The embodiment provides a detection kit, which comprises a reagent 1, a reagent 2 and a reagent 3.
Preparation of reagent 1: 2g of sulfamic acid and 8g of sodium chloride are added into a mortar, fully ground until all raw materials can pass through an 80-target standard sieve, and then sub-packaged into 0.2g of each tube, and vacuumized or sealed by inert gas.
Preparation of reagent 2: ammonium molybdate 0.5g was dissolved in 5mL of water.
Preparation of reagent 3: oxalic acid 1g and ascorbic acid 4g were dissolved in 10mL of water.
Preparing phosphate standard solutions with the concentration of 0mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L, 1mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L and 500mg/L by adopting sodium dihydrogen phosphate stock solution, taking 1-5 ml of each phosphate standard solution, respectively adding the phosphate standard solutions into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, and developing for 1-5 min, wherein the result is shown in figure 4. The sample adding sequence of the reagent is changed, so that the interference of elements such as phosphorus cannot be eliminated.
Example 4
The embodiment provides a detection kit, which comprises a reagent 1, a reagent 2 and a reagent 3.
Preparation of reagent 1: to each tube was added 0.1M hydrochloric acid solution.
Preparation of reagent 2: ammonium molybdate 0.5g was dissolved in 5mL of water.
Preparation of reagent 3: oxalic acid 1g and ascorbic acid 4g were dissolved in 10mL of water.
And (3) detection: preparing silicate standard solutions with different concentrations by adopting a silicon dioxide stock solution, taking 1-5 ml of each silicate standard solution, respectively adding into the reagent 1, shaking uniformly, then adding 1-5 drops of reagent 2, shaking uniformly, then adding 1-5 drops of reagent 3, shaking uniformly, and developing for 1-5 min, wherein the result is shown in figure 5. Other acids can meet the requirements, but sulfuric acid, hydrochloric acid and the like are liquid acids, have strong corrosiveness and are not easy to transport, so the invention does not select liquid acids.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A silicate detection reagent, characterized in that the detection reagent comprises a reagent 1, a reagent 2 and a reagent 3;
The reagent 1 comprises a strong acid reagent and a weighting agent, wherein the mass ratio of the strong acid reagent to the weighting agent is (1-10): 2-10;
The reagent 2 comprises molybdate and water, wherein the mass volume ratio (g: mL) of the molybdate to the water is (1-50): 1-50;
The reagent 3 comprises masking agent, reducing agent and water, wherein the mass volume ratio (g: g: mL) of the masking agent to the reducing agent to the water is (2-30): 10-50): 1-100.
2. The detection reagent according to claim 1, wherein the strongly acidic reagent is selected from one or more of sulfamic acid, citric acid, glycolic acid, benzenesulfonic acid, substituted benzenesulfonic acid, trichloroacetic acid;
The molybdate comprises one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
the masking agent comprises one or more of citric acid, oxalic acid, tartaric acid and EDTA;
The reducing agent comprises one or more of ferrous sulfate, ascorbic acid and stannic chloride;
The weighting agent includes one or more of sodium chloride, sodium sulfate, potassium sulfate.
3. The reagent according to claim 2, wherein the substituent of the substituted benzenesulfonic acid is selected from the group consisting of C1-C4 alkyl, chlorine, bromine and iodine;
Preferably, the substituted benzene sulfonic acid comprises o-C1-C4 alkyl benzene sulfonic acid, m-C1-C4 alkyl benzene sulfonic acid, p-C1-C4 alkyl benzene sulfonic acid, o-chloro benzene sulfonic acid, m-chloro benzene sulfonic acid, p-chloro benzene sulfonic acid, o-bromo benzene sulfonic acid, m-bromo benzene sulfonic acid and p-bromo benzene sulfonic acid;
Preferably, the substituted benzenesulfonic acid is selected from p-toluenesulfonic acid.
4. The detection reagent according to claim 1, wherein the strongly acidic reagent is selected from sulfamic acid;
The molybdate is selected from ammonium molybdate;
the masking agent is selected from oxalic acid;
The reducing agent is selected from ascorbic acid;
the weighting agent is selected from sodium chloride.
5. A silicate detection kit, comprising the detection reagent of claim 1.
6. The test kit of claim 5, further comprising a standard colorimetric card.
7. The method for preparing the detection kit as claimed in claim 5, comprising the steps of:
preparation of reagent 1: according to the proportion of claim 1, the strongly acidic reagent and the weighting agent are fully ground, the ground mixed components can pass through an 80-target standard sieve, and after sub-packaging, vacuumizing or inert gas sealing is carried out;
preparation of reagent 2: according to the proportion of claim 1, molybdate is dissolved in water;
preparation of reagent 3: according to the formulation of claim 1, the masking agent and the reducing agent are dissolved in water.
8. The method according to claim 7, wherein the reagent 1 is dispensed in an amount of 0.1 to 0.5g per tube.
9. The method of claim 7, further comprising the step of preparing a standard colorimetric card: preparing silicate standard solutions with the concentration of 0mg/L, 2.0mg/L, 5.0mg/L, 10.0mg/L, 20mg/L, 50mg/L, 100mg/L, 200mg/L, 500mg/L and 1000mg/L by adopting a silicon dioxide stock solution, taking 1-5 ml of each silicate standard solution, respectively adding the silicate standard solutions into the reagent 1 of claim 7, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, and developing for 1-5 min to obtain the standard colorimetric card.
10. A method for detecting silicate is characterized in that the detection is carried out by adopting the detection kit as claimed in claim 5, and comprises the following steps: adding 1-5 mL of water sample to be detected into the reagent 1, shaking uniformly, then adding 1-5 drops of the reagent 2, shaking uniformly, then adding 1-5 drops of the reagent 3, shaking uniformly, developing for 1-5 min, comparing with a standard colorimetric card, and determining the concentration of silicate in the water sample to be detected.
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