Composition for rapidly detecting copper ions in industrial water
By using compositions of PH regulators, PH stabilizers and identification detection reagents, copper ions in water samples are displayed using chelating agents such as iminodisuccinic acid, which solves the problems of long detection time, large errors and large usage limitations in the prior art, and achieves fast and accurate copper ion detection.
Patent Information
- Application Number
- CN202510254681.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-05
- Publication Date
- 2025-05-30
AI Technical Summary
The method used in the prior art to detect copper ions in industrial water has a long detection time, large errors, and has great limitations in use, making it difficult to make fast and accurate qualitative quantitative judgments.
Using a composition including a PH regulator, a PH stabilizer and an identification detection reagent, the identification detection reagent consists of a color developer, a stabilizer and an anti-interference agent, and the copper ions in the water sample are displayed by chelating agents such as iminodisuccinic acid to achieve rapid detection.
A rapid qualitative and quantitative detection of copper ions in industrial water is achieved, with a detection time of 5 minutes, a qualitative detection time of 30 seconds, and a detection range of 1mg/kg-3%, while effectively avoiding interference from other metals.
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Figure CN120064265A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of water detection, and specifically, to a composition for rapidly detecting copper ions in industrial water. Background Art
[0002] In recent years, with the development of social economy, a large amount of industrial and agricultural wastewater and domestic sewage have been discharged, causing a certain degree of damage to the entire water environment. Coupled with the improper exploitation and utilization of mineral resources and rainwater scouring, a large amount of heavy metals are washed away with soil and water, further exacerbating the heavy metal pollution of fresh water and even marine water environment, resulting in a certain degree of heavy metal pollution problems in most water bodies in real life. In the process of the food chain development, it may ultimately lead to human intake of foods and liquids containing heavy metal substances, affecting people's physical health.
[0003] Therefore, before discharging industrial water, it is necessary to detect copper ions in industrial water to determine that the discharged wastewater does not contain excessive copper ion heavy metal components. In the prior art, the methods for detecting copper ion components in industrial water include ICP-MS method, cuprizone colorimetry, and chemical titration method. Among the above methods, the chemical titration method is suitable for the determination of a large amount of copper ions, but has a large error at low concentrations. The colorimetry method requires the use of organic phase extraction, and the operation process is relatively cumbersome. The ICP-MS method has high precision, but requires the support of precision instruments. In addition, a common disadvantage of the three methods is that the detection time is long, and the use limitations are large, which is not convenient for priority qualitative judgment, and the use scenarios are greatly limited.
[0004] In the prior art, CN113504190B, a rapid detection method and reagent for trace copper in water, uses sodium thiosulfate or thiourea as a masking agent, water-soluble porphyrin as a chromogenic agent, at least one of citric acid, sodium citrate, succinic acid, benzenesulfonic acid, and borax as a buffer, and at least one of cysteine, hydroxylamine hydrochloride, hydroxylamine sulfate, potassium iodide, ascorbic acid, and sodium ascorbate as a catalyst to form a method for detecting copper ions, which can achieve the determination of copper ions within 10 minutes.
[0005] For the detection method of ultra-trace copper ions in water disclosed in Chinese Patent Publication No. CN113376153B, 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline is used as a chromogenic complexing agent, and a polyethersulfone filter membrane is used as a material for enriching and separating the complex, providing a standard colorimetric card and detection method for rapid detection of copper ions, achieving a copper ion concentration of 1×10 -10Horizontal detection ability, with a method sensitivity comparable to that of large analytical instruments. For a rapid copper ion detection test strip for water bodies and its usage method disclosed in Chinese Patent Publication No. CN117451699A, a detection test strip is prepared by a self-assembled silk peptide anthocyanin complex, and rapid detection of copper ions can be achieved through color change. Although the above-mentioned solutions have all achieved the determination of copper ions, they all have the disadvantages of difficult availability of test materials, high prices, and difficult preservation. Although they have certain advantages in detection accuracy or detection speed, they still do not have practical value. Summary of the Invention
[0006] This patent invents a composition for rapidly detecting copper ions in industrial water, which solves the problems of slow copper ion detection, large fluctuations in detection methods, and great limitations in use in the prior art.
[0007] The technical solution of the present invention is as follows: A composition for rapidly detecting copper ions in industrial water includes:
[0008] A pH regulator, a pH stabilizer, and an identification and detection reagent;
[0009] Among them, the identification and detection reagent includes: 90 - 95 parts of a color developer, 1 - 6 parts of a stabilizer, and 4 parts of an anti-interference agent.
[0010] Further, the color developer in the identification and detection reagent is one or a mixture of several of iminodisuccinic acid, sodium iminodisuccinate, and potassium iminodisuccinate. The dry basis purity of the color developer > 97.0%, and it does not contain maleic acid (cis or trans) or aspartic acid (D-type or L-type).
[0011] Further, the stabilizer in the identification and detection reagent is one of water-soluble starch, chitosan, chitosan oligosaccharide, and modified sodium salt of cyclodextrin, and the stabilizer can be quickly dissolved in cold water;
[0012] Among them, water-soluble starch and cyclodextrin are modified sodium salt products, and the degree of alkaline modification > 75%;
[0013] Among them, chitosan and chitosan oligosaccharide are highly deacetylated products and modified sodium salt products, with a degree of deacetylation > 98% and a degree of alkaline modification > 75%.
[0014] Further, the anti-interference agent is a chelating agent that does not have a specific color reaction with copper ions and has a shielding effect on interfering ions, and one of diethanolamine and triethanolamine or a mixture of diethanolamine and triethanolamine can be selected.
[0015] Further, the pH stabilizer is a buffer solution with a pH of 2.0 - 6.0.
[0016] Further, the pH regulator is an inorganic acid solution, preferably hydrochloric acid solution, nitric acid solution or sulfuric acid solution, with a mass concentration of 5-15%.
[0017] Further, when the pH regulator, the pH stabilizer and the identification and detection reagent are used for laboratory determination of copper ions in water samples, they should be stored separately in sealed containers, and the three substances of the identification and detection reagent should also be stored separately in sealed containers;
[0018] When the pH regulator, the pH stabilizer and the identification and detection reagent are used for determination of copper ions in on-site water samples, they should be stored separately in sealed form in a kit / bottle, and the identification and detection reagent is stored after being mixed in proportion.
[0019] Further, during the water sample detection process, the pH regulator, the pH stabilizer and the identification and detection reagent are used in the order of addition during the detection process.
[0020] Further, the preparation method of the identification and detection reagent: Add the color developer, the stabilizer and the anti-interference agent into an open container in proportion, add an appropriate amount of water, and ultrasonically dissolve it into a solution of 0.1-1.5 M (calculated based on the color development reagent) for standby. The solid form of the identification and detection reagent needs to be crushed to a particle size of 3-5 μm by a high-hardness pulverizer.
[0021] Further, the composition for rapid detection of copper ions in industrial water can be used for qualitative and quantitative determination of copper ions in copper-containing water in the laboratory and on-site, and is applicable to the detection of water samples with a copper ion detection concentration of 1 mg / kg - 3%.
[0022] The working principle and beneficial effects of the present invention are as follows:
[0023] In the present invention, when it is necessary to detect copper ions in a water sample, the present application prepares an identification and detection reagent, adds the pH regulator, the pH stabilizer and the identification and detection reagent to the water sample, and uses chelating agents such as iminodisuccinic acid to display the copper ions in the water sample. The general quantitative detection time is 5 minutes, the qualitative detection time is 30S, the detection range is 1 mg / kg - 3%, and at the same time, the interference of other metals can be effectively avoided. The present application is mainly used for qualitative / quantitative detection of copper ions in the water environment, and can also be used for process control during the production of copper compounds, or as a rapid identification of the water quality after copper-containing water treatment.
[0024] In the present invention, the invented reagent can be stored in a reagent bottle and determined by potentiometric titration method, and can also be applied on-site in the form of a kit / bottle, thus reducing the requirements for qualitative and quantitative judgment in the application scenario. At the same time, this method has a rapid detection speed and can be set to a multi-gradient detection range, so it is more suitable for use in the corresponding scenario. Description of the Drawings
[0025] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
[0026] Figure 1 It is a schematic diagram of the water sample detection method of the present invention;
[0027] Figure 2 It is a comparison schematic diagram of the qualitative colorimetric solution of 0.5%-3% in the present invention;
[0028] Figure 3 It is a comparison schematic diagram of the qualitative colorimetric solution of 0.05%-1% in the present invention;
[0029] Figure 4 It is a comparison schematic diagram of the qualitative colorimetric solution of 5-500 ppm in the present invention;
[0030] Figure 5 It is a schematic diagram of the identification detection reagent, pH regulator and pH stabilizer in the present invention. Specific Embodiments
[0031] Next, in conjunction with the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
[0032] Please refer to Figures 1 to 5 ;
[0033] Example 1, 1.0M concentration
[0034] A composition for rapidly detecting copper ions in industrial water is operated as follows:
[0035] Preparation of the identification detection reagent: Place 358.43 g of sodium iminodisuccinate, 4.18 g of sodium salt of modified starch, and 14.37 g of triethanolamine in a 1 L four-necked flask, stir evenly, add 623.02 g of pure water, start stirring, and dissolve at 45 °C with stirring to obtain the identification detection reagent Ⅰ. In the above scheme, the dry basis content of sodium iminodisuccinate is 98.5%, the water content is 4.52%, it does not contain maleic acid (cis or trans) or aspartic acid (D-type or L-type), the alkaline modification degree of the sodium salt of modified starch is 95%, the water content is 15.05%, the triethanolamine is of analytical grade, and the content is 98.80%. The above identification detection reagent is detected, and the solution concentration is 1M concentration of the identification detection reagent. The above identification detection reagent Ⅰ is sub-packed in 5 mL and 10 mL reagent bottles to obtain the portable identification detection reagent Ⅰ, which can be used for qualitative and quantitative detection of copper content in water containing 1.0-2.0% copper ions.
[0036] Preparation of pH regulator: Referring to the method for preparing acid-base solutions in the Practical Handbook for Laboratory Technicians (Third Edition), prepare a 10% (w / w) sulfuric acid solution. The pH regulator is dispensed into reagent bottles with a volume of 1 - 10 mL, thus obtaining the portable pH regulator I, which is used in conjunction with the portable identification and detection reagent I.
[0037] Preparation of pH stabilizer: Select the acetic acid - sodium acetate buffer solution system with a pH of 3.6. The preparation method refers to the method for preparing ordinary buffer solutions in the Practical Handbook for Laboratory Technicians (Third Edition). The pH stabilizer is dispensed into 20 - mL reagent bottles, thus obtaining the portable pH stabilizer I, which is used in conjunction with the portable identification and detection reagent I.
[0038] Example 2, 0.5 M concentration
[0039] A composition for rapid detection of copper ions in industrial water is prepared according to the following procedure:
[0040] Preparation of identification and detection reagent: Place 215.87 g of potassium iminodisuccinate, 9.98 g of sodium salt of cyclodextrin, and 8.85 g of diethanolamine into a 1 - L four - necked flask, stir evenly, add 765.30 g of pure water, start stirring, and dissolve at 40 °C to obtain the identification and detection reagent II. In the above - mentioned scheme, the dry - basis content of potassium iminodisuccinate is 98.02%, the water content is 5.22%, and it does not contain maleic acid (cis or trans) or aspartic acid (D - type or L - type). The degree of alkaline modification of sodium cyclodextrin is 90%, the water content is 12.65%, and diethanolamine is of analytical purity with a content of 98.50%. Detect the above - mentioned identification and detection reagent. The solution concentration of the identification and detection reagent is 0.5 M. Dispense the above - mentioned identification and detection reagent II into 5 - mL and 10 - mL reagent bottles, thus obtaining the portable identification and detection reagent II, which can be used for qualitative and quantitative detection of copper content in water containing 0.2 - 1.0% copper ions.
[0041] Preparation of pH regulator: Referring to the method for preparing acid - base solutions in the Practical Handbook for Laboratory Technicians (Third Edition), prepare a 10% (w / w) hydrochloric acid solution. The remaining operations are the same as those for preparing the pH regulator in Example 1, thus obtaining the portable pH stabilizer II, which is used in conjunction with the portable identification and detection reagent II.
[0042] Preparation of pH stabilizer: The same as the preparation of the pH stabilizer in Example 1, thus obtaining the portable pH stabilizer II, which is used in conjunction with the portable identification and detection reagent II.
[0043] Example 3, 1.5 M concentration
[0044] A composition for rapid detection of copper ions in industrial water is prepared according to the following procedure:
[0045] Preparation of the identification and detection reagent: Place 647.61 g of potassium iminodisuccinate, 29.94 g of sodium salt of cyclodextrin, and a 1:2 mass ratio mixture of diethanolamine and triethanolamine (26.55 g) into a 1 L four-necked flask, stir evenly, add 295.9 g of pure water, start stirring, and stir to dissolve at 40 °C to obtain the identification and detection reagent III. In the above scheme, the dry basis content of potassium iminodisuccinate is 98.02%, the water content is 5.22%, it does not contain maleic acid (cis or trans) or aspartic acid (D-form or L-form), the degree of alkaline modification of sodium cyclodextrin is 90%, the water content is 12.65%, diethanolamine is of analytical purity with a content of 98.50%, and triethanolamine is of analytical purity with a content of 98.80%. Detect the above identification and detection reagent. The solution concentration of the identification and detection reagent is 1.5 M. Package the above identification and detection reagent III into 5 mL and 10 mL reagent bottles to obtain the portable identification and detection reagent III. This reagent can be used for qualitative and quantitative detection of copper content in water containing 2.0 - 3.0% copper ions.
[0046] Preparation of the pH regulator: Refer to the "Practical Handbook for Chemical Analysts" (Third Edition) for the preparation method of acid-base solutions. Prepare a 10% (w / w) nitric acid solution. The remaining operations are the same as those for the preparation of the pH regulator in Example 1 to obtain the portable pH stabilizer III. This reagent is used in conjunction with the portable identification and detection reagent III.
[0047] Preparation of the pH stabilizer: The same as the preparation of the pH stabilizer in Example 1 to obtain the portable pH stabilizer III. This reagent is used in conjunction with the portable identification and detection reagent III.
[0048] Example 4, 0.1 M concentration
[0049] A composition for rapid detection of copper ions in industrial water is carried out according to the following operations:
[0050] Preparation of the identification and detection reagent: Place 35.84 g of sodium iminodisuccinate, 0.40 g of modified sodium salt of chitosan oligosaccharide, and 1.44 g of triethanolamine into a 0.25 L four-necked flask, stir evenly, add 62.28 g of pure water, start stirring, and stir to dissolve at 45 °C to obtain the identification and detection reagent IV. In the above scheme, the dry basis content of sodium iminodisuccinate is 98.5%, the water content is 4.52%, it does not contain maleic acid (cis or trans) or aspartic acid (D-form or L-form), the degree of deacetylation of the modified sodium salt of chitosan oligosaccharide is 98.62%, the degree of alkaline modification is 90%, the water content is 10.05%, and triethanolamine is of analytical purity with a content of 98.80%.
[0051] For the detection of the above identification and detection reagent, the identification and detection reagent with a solution concentration of 0.1 M was used, and the remaining operations were the same as those in Example 1, thus obtaining the portable identification and detection reagent Ⅳ, which can be used for the qualitative and quantitative detection of copper content in water containing copper ions at 1.0 mg / kg - 0.2%.
[0052] Preparation of pH regulator: The same as the pH regulator in Example 1, thus obtaining the portable pH regulator Ⅳ, which is used in conjunction with the portable identification and detection reagent Ⅳ.
[0053] Preparation of pH stabilizer: The same as the preparation operation of the H stabilizer in Example 1, thus obtaining the portable pH stabilizer Ⅳ, which is used in conjunction with the portable identification and detection reagent Ⅳ.
[0054] Example Five - Solid Scheme
[0055] A composition for the rapid detection of copper ions in industrial water is prepared according to the following operations:
[0056] Preparation of identification and detection reagent: 966.19 g of iminodisuccinic acid, 10.50 g of sodium salt of modified starch, and 40.50 g of triethanolamine were placed in a mixer and stirred evenly. The above mixture was then placed in a high - speed grinder at 9000 r / min for [time not specified in the original, assumed to be a typo and should be 'for a certain time'], thus obtaining the identification and detection reagent Ⅴ. In the above scheme, the dry - basis content of iminodisuccinic acid is 99.64%, the water content is 1.32%, and it does not contain maleic acid (cis or trans) or aspartic acid (D - type or L - type). The degree of alkaline modification of the sodium salt of modified starch is 75.14%, the water content is 5.12%, and the triethanolamine is of analytical purity with a content of 98.80%. For the detection of the above identification and detection reagent, the identification and detection reagent with a concentration of 3.75 M. The above identification and detection reagent Ⅴ was packaged in kits of 2.5 g and 5.0 g, thus obtaining the portable identification and detection reagent Ⅳ, which can be used for the qualitative and quantitative detection of copper content in water containing copper ions at 2.0 - 3.0%.
[0057] Preparation of pH regulator: The same as the pH regulator in Example 1, thus obtaining the portable pH regulator Ⅴ, which is used in conjunction with the portable identification and detection reagent ⅣⅤ.
[0058] Preparation of pH stabilizer: The same as the preparation operation of the H stabilizer in Example 1, thus obtaining the portable pH stabilizer Ⅴ, which is used in conjunction with the portable identification and detection reagent Ⅴ.
[0059] Comparative Example Five - Lack of Stabilizer
[0060] A composition for the rapid detection of copper ions in industrial water is prepared according to the following operations:
[0061] Preparation of the identification and detection reagent: Place 358.43 g of iminodisuccinic acid sodium salt and 14.37 g of triethanolamine in a 1 L four-necked flask, stir evenly, add 627.20 g of pure water, start stirring, and stir and dissolve at 45 °C to obtain the identification and detection reagent VI. The remaining operations are the same as those in Example 1.
[0062] Comparative Example 2 lacks an anti-interference agent
[0063] A composition for rapid detection of copper ions in industrial water is carried out according to the following operations:
[0064] Preparation of the identification and detection reagent: Place 358.43 g of iminodisuccinic acid sodium salt and 4.18 g of sodium salt of modified starch in a 1 L four-necked flask, stir evenly, add 637.39 g of pure water, start stirring, and stir and dissolve at 45 °C to obtain the identification and detection reagent VII. The remaining operations are the same as those in Example 1.
[0065] The color-developing reagent in Comparative Example 3 is lower than the required ratio
[0066] A composition for rapid detection of copper ions in industrial water is carried out according to the following operations:
[0067] Preparation of the identification and detection reagent: Place 358.43 g of iminodisuccinic acid sodium salt, 6.24 g of sodium salt of modified starch, and 28.74 g of triethanolamine in a 1 L four-necked flask, stir evenly, add 606.59 g of pure water, start stirring, and stir and dissolve at 45 °C to obtain the identification and detection reagent VI. The remaining operations are the same as those in Example 1.
[0068] The color-developing reagent in Comparative Example 4 is higher than the required ratio
[0069] A composition for rapid detection of copper ions in industrial water is carried out according to the following operations:
[0070] Preparation of the identification and detection reagent: Place 358.43 g of iminodisuccinic acid sodium salt, 2.09 g of sodium salt of modified starch, and 7.20 g of triethanolamine in a 1 L four-necked flask, stir evenly;
[0071] Add 632.28 g of pure water, start stirring, and stir and dissolve at 45 °C to obtain the identification and detection reagent VI. The remaining operations are the same as those in Example 1.
[0072] Comparative Example 5 has no pH regulator
[0073] A composition for rapid detection of copper ions in industrial water is carried out according to the following operations:
[0074] The preparation of the identification and detection reagent and the pH stabilizer are the same as those in Example 1, and there is no pH regulator.
[0075] Comparative Example 6 has no pH stabilizer
[0076] A composition for rapid detection of copper ions in industrial water is operated as follows:
[0077] The preparation of the identification detection reagent, pH regulator is the same as that in Example 1, and there is no pH stabilizer.
[0078] Application Example 1 Standard copper ion test
[0079] The above-mentioned identification detection reagents, pH regulators and pH stabilizers obtained in Example 1 and Comparative Examples 1-6 are used for the determination of copper content in water with a standard copper ion content of 1.5%. The preparation method of water with a standard copper ion content of 1.5% is as follows: Dissolve 59.50 g of 98.50% copper sulfate pentahydrate in 940.50 g of water, and use a standard sodium thiosulfate solution to calibrate the copper ion concentration to 1.5004%.
[0080] In this experiment, 10 g of the above standard copper sulfate solution was respectively pipetted into an open bottle, 40 ML of pure water and 1 1-cm date pit-shaped magnet were added, 2 mL of each of the above pH regulators and 20 mL of pH stabilizer were respectively added. After stirring at a speed of 60 r / min for 10 min, a ZDJ-4B type automatic potentiometric titrator was used to titrate with the identification detection reagents obtained in Example 1 and Comparative Examples 1-6. Each treatment was measured 4 times repeatedly. After taking the average value, the above relevant data was sorted out using Word2017, and one-way analysis of variance was performed using the SPSS22.0 data analysis system and the difference significance (t = 0.01) test was performed using the Dunckans method.
[0081] Table 1 Influence of different compositions on the detection of standard copper ions
[0082]
[0083]
[0084] As can be seen from the above table, under the standard copper ion condition, for the detection rate of copper ions, Example 1 has little influence on the detection of copper ions under this condition compared with Comparative Examples 2 and 4, and there is almost no difference. However, the detection rates of copper ions in the remaining treatments all exceed an error of 1%, resulting in a large deviation in detection;
[0085] It should be noted that although no difference in the detection rate between Example 1 and Comparative Examples 2 and 4 was found in this experiment, it is undeniable that this experiment was under standard conditions and only represented the calibration aspect after preparing the copper-containing solution, and did not represent the application aspect in industrial water. Therefore, subsequent experiments will continue to prove in the above-mentioned aspects.
[0086] Application Example 2 Influence of ion interference on detection
[0087] According to the test results of the standard copper ion test in Application Example 1, the above-mentioned identification and detection reagents, pH regulators, and pH stabilizers obtained in the above-mentioned Example 1, Comparative Examples 2 and 4 were used to determine the copper content in water with a copper ion content of 1.5% containing impurity ions. The preparation method of water with a copper ion content of 1.5% containing impurity ions is as follows: ① Dissolve 59.50 g of 98.50% copper sulfate pentahydrate and 1.0 g of 95.62% ferrous sulfate heptahydrate in 939.50 g of water. Calculate that the copper ion concentration is 1.5004% and the iron ion concentration is 0.019%. ② Dissolve 59.50 g of 98.50% copper sulfate pentahydrate and 1.0 g of 98.62% zinc nitrate hexahydrate in 939.50 g of water. Calculate that the copper ion concentration is 1.5004% and the zinc ion concentration is 0.022%. ③ Dissolve 59.50 g of 98.50% copper sulfate pentahydrate and 1.0 g of 98.25% magnesium sulfate monohydrate in 939.50 g of water. Calculate that the copper ion concentration is 1.5004% and the magnesium ion concentration is 0.017%.
[0088] In this experiment, 10 g of each of the above-mentioned copper sulfate solutions was separately pipetted into an open bottle, and the remaining treatments were the same as those in Application Example 1. The ZDJ-4B automatic potentiometric titrator was also used to titrate with the identification and detection reagents obtained in the above-mentioned Example 1, Comparative Examples 2 and 4. Each treatment was measured 4 times repetitively. After calculating the average value, the above relevant data was sorted out using Word 2017, and one-way analysis of variance was performed using the SPSS 22.0 data analysis system, and the significance of differences (t = 0.01) was tested using the Dunckans method.
[0089] Table 2 Influence of different compositions on the detection of copper ions under ion interference conditions
[0090]
[0091]
[0092] As can be seen from the above table, under the interference of impurity ions, the detection rate of copper ions is most affected by the variable-valence transition metal ions represented by iron ions. Among them, significant changes have occurred in the detection rates of Comparative Examples 2 and 4, which also proves the advantages of the composition in detecting copper ions. At the same time, the technicians also found that although the non-variable-valence transition metal ions represented by zinc ions and the alkali metal ions represented by magnesium have a certain influence on the detection rate of copper, their detection rates have not deviated excessively and are still within the detection error range. However, in order to reduce errors, it is still necessary to select this composition to detect copper ions in water containing the above-mentioned ions;
[0093] It should be noted that common calcium ions were not added as interference in this experiment. This was mainly considered because the precipitation problem between calcium ions and sulfate ions would not cause interference. The superiority of the composition was verified in this experiment. Therefore, the detection of industrial copper-containing water will be carried out based on this in the future.
[0094] Application Example 3 Qualitative Detection Experiment
[0095] The composition described in Example 2 was sub-packed for on-site qualitative inspection. The preparation work was as follows: ① Understand the water quality situation at the site: the copper content was unknown, and it might contain a small amount of iron ions. At the same time, the pH was 6.20. ② Select reagent specifications: Select 5 mL and 20 mL of pH regulators, and select two specifications of 5 mL and 10 mL of identification and detection reagents, and carry a colorimetric solution with a standard concentration and pure water.
[0096] Qualitative experiment: Take two portions of the above 10 mL water samples in mineral water bottles. After shaking well with about 40 mL of pure water respectively, continue to add the pH regulator and shake well, and then add 5 mL and 10 mL of the above identification and detection reagents respectively. After standing for 30 S, compare the solution with the standard colorimetric solution. It was found that the copper contents of the above water samples were 0.50% and 0.54% respectively.
[0097] Application Example 4 Quantitative Detection Experiment
[0098] After the water samples in Application Example 3 were treated with sodium sulfide for precipitation, water samples were taken again for testing after treatment. It was expected that the copper ion concentration was lower than 0.2%. Therefore, the composition of Example 4 was selected for testing, and at the same time, the water samples in Application Example 3 were selected for synchronous detection, and the composition of Example 2 was selected for testing.
[0099] This experiment was carried out in the laboratory of Hebei Xietong Chemical Co., Ltd. The experimental conditions were the same as those in Application Example 2. Each treatment was measured 4 times, and the average value was calculated and compared with the ICP data. Then the relevant data was sorted out using Word 2017, and a one-way analysis of variance was performed using the SPSS 22.0 data analysis system, and a significance test of differences (t = 0.01) was carried out using the Dunckans method.
[0100] Table 3 Comparison of Water Sample Detection
[0101] treatment ICP detected amount of composition water sample before treatment / % 0.52a 0.51a water sample after treatment / mg / kg 36.47a 36.25a
[0102] It can be seen from the comparison data of water sample detection in Table 3 that the water samples before and after treatment were detected using ICP and this composition respectively, and there was no significant difference in the results. This proves that this composition can be used for the qualitative / quantitative detection of copper ions in water environment, can also be used for the process control in the production of copper compounds, or as a rapid identification of the water quality after copper-containing water treatment.
[0103] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.
Claims
1. A composition for rapid detection of copper ions in industrial water, characterized in that: include: PH regulators, PH stabilizers and identification and testing reagents; The identification and detection reagent comprises: 90-95 parts of a color developer, 1-6 parts of a stabilizer and 4 parts of an anti-interference agent.
2. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The color developer in the identification and detection reagent is one or a mixture of iminodisuccinic acid, sodium iminodisuccinate, potassium iminodisuccinate, and the color developer has a dry basis purity of >97.0% and does not contain butenedioic acid (cis or trans) or aspartic acid (D or L).
3. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The stabilizer in the identification and detection reagent is one of water-soluble starch, chitosan, chitosan oligosaccharide, and modified sodium salt of cyclodextrin, and the stabilizer can be quickly dissolved in cold water; Wherein, the water-soluble starch and the cyclodextrin are modified sodium salt products, and the degree of alkaline modification is greater than 75%; The chitosan and the chitosan oligosaccharide are highly deacetylated and modified sodium salt products, with a deacetylation degree of more than 98% and an alkaline modification degree of more than 75%.
4. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The anti-interference agent is a chelating agent that does not have a specific color reaction with copper ions and has a shielding effect on interfering ions. One of diethanolamine and triethanolamine or a mixture of diethanolamine and triethanolamine can be selected.
5. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The pH stabilizer is a buffer solution with a pH of 2.0-6.
0.
6. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The pH regulator is an inorganic acid solution, preferably a hydrochloric acid solution, a nitric acid solution or a sulfuric acid solution, with a mass concentration of 5-15%.
7. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: The pH regulator, the pH stabilizer and the identification and detection reagent should be stored separately in a sealed container when the copper ions in the water sample are determined in the laboratory, and the three substances of the identification and detection reagent should also be stored separately in a sealed container; The pH regulator, the pH stabilizer and the identification and detection reagent should be stored separately in a sealed form in the form of a test kit / bottle when determining copper ions in an on-site water sample, wherein the identification and detection reagent is stored after being mixed in proportion.
8. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: During the water sample detection process, the pH regulator, the pH stabilizer and the identification detection reagent are used in the detection process in the order of addition.
9. A composition for rapid detection of copper ions in industrial water according to any one of claims 1 to 8, characterized in that: The preparation method of the identification and detection reagent is as follows: the color developer, the stabilizer and the anti-interference agent are added into an open container in proportion, an appropriate amount of water is added, and ultrasonically dissolved into a 0.1-1.5M (based on the color developer) solution for use. The solid form of the identification and detection reagent needs to be crushed with a high-hardness grinder to a particle size of 3-5μm.
10. A composition for rapid detection of copper ions in industrial water according to claim 1, characterized in that: It is suitable for testing water samples with copper ion concentration of 1mg / kg-3%.
Citation Information
Patent Citations
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