WO2025129388A1 - 一种磷酸根的检测试剂、检测试剂盒和检测方法 - Google Patents

一种磷酸根的检测试剂、检测试剂盒和检测方法 Download PDF

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WO2025129388A1
WO2025129388A1 PCT/CN2023/139465 CN2023139465W WO2025129388A1 WO 2025129388 A1 WO2025129388 A1 WO 2025129388A1 CN 2023139465 W CN2023139465 W CN 2023139465W WO 2025129388 A1 WO2025129388 A1 WO 2025129388A1
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reagent
agent
detection
molybdate
acid
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盛宗海
胡德红
郑海荣
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Shenzhen Institute of Advanced Technology of CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—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
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • 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

Definitions

  • the invention belongs to the technical field of analytical chemistry, and in particular relates to a detection reagent, a detection kit and a detection method for phosphate radical.
  • Phosphorus is one of the elements necessary for biological growth, but too high a phosphorus content in water will interfere with the coagulation process in the water plant. Phosphorus is a key element required for algae growth. Excessive phosphorus content will cause excessive growth of algae, eutrophication of water quality, and affect the ecological balance of water bodies. Generally, the phosphate content in natural water is not high, and its main source is industrial wastewater from industries such as domestic sewage, fertilizers, smelting, organophosphorus pesticides and synthetic detergents. Phosphorus is one of the important indicators for evaluating water quality.
  • the determination of phosphate is commonly done by weight method, titration method, ion chromatography, spectrophotometry, atomic absorption spectrophotometry, Raman spectroscopy, etc.
  • spectrophotometry is the most commonly used method, which is widely used in the water quality testing industry. Its advantages are simple, fast, accurate, and there are complete standard analysis and determination methods. However, this method requires a large amount of reagents, heavy environmental pollution, cumbersome and time-consuming, high professional requirements, and emergency difficulties, which limits its application in rapid detection.
  • the advantage of the weight method is that it has high accuracy and is still recommended as a standard method at home and abroad.
  • the advantages of the rapid test kit method are that it is cheap, only a few hundred yuan is needed to test dozens of times, it is fast, only 5 minutes to get the result, and it is light and convenient. Its disadvantage is that it is not accurate enough and can only estimate a large range of values.
  • the existing detection of phosphate content in water systems often uses the ammonium molybdate spectrophotometry method, which includes the molybdenum yellow method or the molybdenum blue method.
  • the ammonium molybdate spectrophotometry method is simple to operate and low in cost.
  • the molybdenum yellow method is a direct determination of phosphovanadomolybdenum yellow heteropoly acid formed by the reaction of phosphoric acid with vanadic acid and molybdic acid.
  • a liquid solution of a strong acid such as sulfuric acid or nitric acid is generally used.
  • the liquid solution of the strong acid has high requirements for transportation, cumbersome operation, unsafe, and certain risks.
  • the molybdenum blue method is to react active phosphate with molybdate to form phosphomolybdenum yellow, and use a reducing agent to reduce phosphomolybdenum yellow to phosphomolybdenum blue.
  • the color depth is proportional to the concentration of effective phosphorus, and it conforms to the Lambert-Beer law within a certain range, so it can be determined by colorimetry.
  • the reducing agents used include stannous chloride, ascorbic acid, hydrazine sulfate and sulfite.
  • the Chinese patent with publication number CN106442511A discloses a phosphate rapid detection kit and detection method.
  • the detection kit and the detection method of the supporting test paper can make the entire detection process of phosphate only take 2 minutes, greatly simplify the process, and the shelf life can reach two years.
  • the disadvantage is that the interference of elements such as arsenic and silicon cannot be eliminated.
  • a liquid solution of a strong acid such as sulfuric acid or nitric acid is used.
  • the liquid solution of the strong acid has high requirements for transportation, cumbersome operation, unsafe, and certain dangers.
  • the purpose of the present invention is to overcome the shortcomings and deficiencies of the prior art and to provide a phosphate detection reagent, a detection kit and a detection method.
  • the present invention provides a phosphate detection reagent, the detection reagent comprising reagent A and reagent B;
  • the reagent A comprises a strong acid reagent, a molybdate and a weighting agent, wherein the mass ratio of the strong acid reagent, the molybdate and the weighting agent is (2-98): (0.2-20.0): (0-50.0);
  • the reagent B comprises a strong acidic reagent, a masking agent, a reducing agent, an accelerating agent and a weighting agent, wherein the mass ratio of the strong acidic reagent, the masking agent, the reducing agent, the accelerating agent and the weighting agent is (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0).
  • the mass ratio of the strong acid reagent, the molybdate and the weighting agent in the reagent A is (5-10): (0.5-2.0): (0-5.0);
  • the mass ratio of the strong acid reagent, the masking agent, the reducing agent, the speed increasing agent and the weight increasing agent in the reagent B is (5-10): (1.0-5.0): (0.5-1.5): (0.1-0.5): (0-5.0).
  • the mass ratio of the strong acid reagent, the molybdate and the weighting agent in the reagent A is 7:1:2;
  • the mass ratio of the strong acid reagent, the masking agent, the reducing agent, the speed increasing agent and the weight increasing agent in the reagent B is 5:1:1:0.2:2.
  • the strong acidic agent is selected from one or more of sulfamic acid, citric acid, and glycolic acid;
  • the molybdate includes one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
  • the masking agent includes one or more of potassium sodium tartrate, citric acid, oxalic acid, tartaric acid, and EDTA;
  • the reducing agent includes at least one of ascorbic acid, hydrazine sulfate, tin dichloride, sodium chloride-stannous chloride, hydrazine sulfate, 1-amino-2-tetraphenol-4-sulfonic acid, p-aminophenol sulfate, hydroquinone, thiophenylamine, ammonium ferrous sulfate-fructose, ammonium ferrous sulfate-glucose, sodium pyrosulfite, metol, sodium formaldehyde bisulfite, titanium trichloride, sulfite-iron salt, ammonium ferrous sulfate, sodium sulfite, sodium bisulfite and antimony (III);
  • the speed increasing agent is at least one of potassium antimony tartrate and bismuth nitrate;
  • the weighting agent includes one or more of sodium chloride, sodium sulfate and potassium sulfate.
  • the strong acid reagent is aminosulfonic acid
  • the molybdate is sodium molybdate
  • the masking agent is potassium sodium tartrate
  • the reducing agent is ascorbic acid
  • the speed increasing agent is potassium antimony tartrate
  • the weighting agent is sodium chloride.
  • Another aspect of the present invention provides a phosphate detection kit, which comprises a reagent A and a reagent B, and a standard colorimetric card.
  • Another aspect of the present invention provides a method for preparing the above detection kit, comprising the steps of:
  • Preparation of reagent A Grind the strong acid reagent, molybdate and weighting agent fully according to the above mass ratio, and the mixed components after grinding can pass through an 80-mesh standard sieve. After packaging, vacuumize or seal with inert gas;
  • Preparation of reagent B Grind the strong acid reagent, masking agent, reducing agent, weighting agent and speed increasing agent fully according to the above mass ratio, and the mixed components after grinding can pass through an 80-mesh standard sieve. After packaging, vacuumize or seal with inert gas;
  • Preparation of standard colorimetric card prepare phosphate standard solutions with concentrations of 0 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20 mg/L, 50 mg/L, 100 mg/L, 200 mg/L, 500 mg/L, and 1000 mg/L, take 1-5 mL of various phosphate standard solutions, add the reagent A respectively, shake well, then add reagent B, shake well, and after color development for 1-5 minutes, a standard colorimetric card is obtained.
  • reagent A and reagent B are packaged into 0.1-0.5 g per tube.
  • the present invention also provides a method for detecting phosphate, which uses the detection kit for detection, comprising the steps of: adding 1-5 mL of a water sample to be tested into reagent A, shaking well, then adding reagent B, shaking well, and after 1-5 minutes, comparing with a standard colorimetric card to determine the concentration of phosphate in the water sample to be tested.
  • the detection kit of the present invention should be stored in a cool and dry place, preferably at a storage temperature below 26°C. If the temperature is higher than 25°C, the unused test paper bag should be stored in the fresh-keeping layer of the refrigerator and stored in a light-proof and moisture-proof package.
  • the effective use period of the detection kit of the present invention is about one year.
  • the phosphate detection method of the present invention is based on the phosphomolybdenum blue method, which is a fast and flexible phosphate detection method that does not require any equipment and has low production and use costs.
  • the kit of the present invention has no special environmental requirements, no special three waste pollution, low cost, simple detection steps, no interference, more accurate determination, short color development time and strong mobility.
  • the present invention is different from traditional methods or Compared with other determination forms, it is more convenient to use and does not require specialized technicians to perform the determination.
  • the reagents used in the present invention are all common chemical reagents, which are safe, reliable and inexpensive. It has a wide range of applications and can be used to determine the phosphate content of water bodies such as chemical wastewater, surface water, urban sewage recycling-landscape environment water and urban miscellaneous water, especially in the monitoring of phosphate in the field of environmental protection.
  • the present invention eliminates the interference of elements such as arsenic and silicon by adding more acid to reagent A. Phosphate in the water sample to be tested reacts with molybdate in reagent A to generate light yellow phosphomolybdic yellow, and then the masking agent in reagent B added can chelate the molybdenum in molybdate, thereby improving the detection sensitivity.
  • FIG. 1 is a standard colorimetric card of the detection kit of Example 1.
  • FIG2 is the color development result of Example 1
  • FIG3 is the color development result of Example 2.
  • FIG4 is the color development result of Example 3.
  • FIG. 5 is the color development result of Example 4.
  • This embodiment provides a phosphate detection kit, which includes reagent A, reagent B and a standard colorimetric card.
  • the specific preparation method is as follows:
  • reagent A According to the mass ratio of strongly acidic reagent, molybdate and weighting agent (2-98): (0.2-20.0): (0-50.0), prepare strongly acidic reagent, molybdate and weighting agent, add the above components into a mortar, fully grind until all raw materials can pass through an 80-mesh standard sieve, and then pack into 0.1-0.5 grams per tube, evacuate or seal with inert gas.
  • the mass ratio of strongly acidic reagent, molybdate and weighting agent is (5-10): (0.5-2.0): (0-5.0).
  • reagent B According to the mass ratio of strong acid reagent, masking agent, reducing agent, speed-increasing agent and weighting agent of (2-98): (1.0-30.0): (0.5-50.0): (0.1-50.0): (0-50.0), prepare strong acid reagent, masking agent, reducing agent, speed-increasing agent and weighting agent, add the above components into a mortar, grind them thoroughly until all raw materials can pass through an 80-mesh standard sieve, and then pack them into 0.1-0.5 g per tube, and evacuate or seal them with inert gas.
  • the strong acid reagent The mass ratio of the agent, masking agent, reducing agent, speed increasing agent and weight increasing agent is (5-10): (1.0-5.0): (0.5-1.5): (0.1-0.5): (0-5.0).
  • Preparation of standard colorimetric card Use phosphate stock solution (1000 mg/L) to prepare phosphate standard solutions with concentrations of 0 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20 mg/L, 50 mg/L, 100 mg/L, 200 mg/L, 500 mg/L, and 1000 mg/L. Take 1-5 mL of various phosphate standard solutions, add solid reagent A respectively, shake well, then add solid reagent B, shake well, and the color will be basically stable after 1-5 minutes of color development to prepare a standard colorimetric card.
  • the strong acidic agent is selected from one or more of aminosulfonic acid, citric acid, and glycolic acid;
  • Molybdate includes one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
  • the masking agent includes one or more of potassium sodium tartrate, citric acid, oxalic acid, tartaric acid, and EDTA, and the masking agent is used to chelate molybdenum in molybdate;
  • the reducing agent includes at least one of ascorbic acid, hydrazine sulfate, tin dichloride, sodium chloride-stannous chloride, hydrazine sulfate, 1-amino-2-tetraphenol-4-sulfonic acid, p-aminophenol sulfate, hydroquinone, thiophenylamine, ammonium ferrous sulfate-fructose, ammonium ferrous sulfate-glucose, sodium pyrosulfite, metol, sodium formaldehyde hyposulfite, titanium trichloride, sulfite-iron salt, ammonium ferrous sulfate, sodium sulfite, sodium bisulfite and antimony (III);
  • the speed increasing agent is at least one of potassium antimony tartrate and bismuth nitrate;
  • the weighting agent includes one or more of sodium chloride, sodium sulfate, and potassium sulfate.
  • the weighting agent facilitates the weighing of reagent A and reagent B.
  • the prepared test kit should be stored in a cool and dry place, preferably below 26°C. If the temperature is higher than 25°C, the unused test paper bag should be stored in the fresh-keeping layer of the refrigerator and stored in a light-proof and moisture-proof package.
  • the present embodiment further provides a method for detecting phosphate, which is detected using the prepared detection kit, comprising the steps of: adding 1-5 mL of the water sample to be tested to reagent A, shaking well, then adding reagent B, shaking well, and after 1-5 minutes, if phosphate is present in the water, a blue-green color is displayed, and the depth of the color is related to the concentration of phosphate in the water.
  • the concentration of phosphate in the water sample to be tested is determined by comparing with a standard colorimetric card.
  • This embodiment provides a detection kit, the raw materials of each component of reagent A are: 7g aminosulfonic acid, 1g sodium molybdate, and 2g sodium chloride.
  • the raw materials of each component of reagent B are: 5g aminosulfonic acid, 1g potassium sodium tartrate, 1g ascorbic acid, 0.2g potassium antimony tartrate, and 2g sodium chloride.
  • Reagent A and reagent B are prepared according to the above method, and reagent A and reagent B are evenly packaged into 0.2g per tube.
  • phosphate stock solution 1000 mg/L to prepare concentrations of 0 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/L, 1 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20 mg/L, 30 mg/L, 50 mg/L, 100 mg/L, 200 mg/L, 500 mg/L, 1000 mg/L phosphate standard solution, take 1-5 mL of various phosphate standard solutions, add solid reagent A respectively, shake well, then add solid reagent B, shake well, and the color is basically stable after 1-5 minutes of color development.
  • the color development results of phosphate standard solutions of different concentrations are shown in Figure 2.
  • the standard colorimetric card prepared based on the reagent A and reagent B in the kit of this embodiment is shown in Figure 1.
  • This embodiment provides a detection kit
  • the raw materials of each component of reagent A are: 1g aminosulfonic acid, 1g sodium molybdate, and 8g sodium chloride.
  • the raw materials of each component of reagent B are: 1g aminosulfonic acid, 1g potassium sodium tartrate, 1g ascorbic acid, 0.2g potassium antimony tartrate, and 7g sodium chloride.
  • Reagent A and reagent B are prepared according to the above method, and reagent A and reagent B are evenly packaged into 0.2g per tube.
  • Silica stock solution 1000 mg/L was used to prepare 0 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/L, 1 mg/L, 2.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20 mg/L, 30 mg/L, 50 mg/L, 100 mg/L silica standard solutions.
  • 1-5 mL of various silica standard solutions were added to solid reagent A, shaken well, and then solid reagent B was added, shaken well, and the color was basically stable after 1-5 minutes of color development.
  • Figure 3 This shows that the kit cannot eliminate the interference of elements such as silicon by reducing the concentration of acid.
  • This embodiment provides a detection kit, the raw materials of each component of reagent A are: 7g aminosulfonic acid, 1g sodium molybdate, and 2g sodium chloride.
  • the raw materials of each component of reagent B are: 5g aminosulfonic acid, 0.2g potassium antimony tartrate, and 4g sodium chloride.
  • Reagent A and reagent B are prepared according to the above method, and reagent A and reagent B are evenly packaged into 0.2g per tube.
  • Silica stock solution 1000 mg/L was used to prepare 0.25 mg/L, 0.5 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L, 8.0 mg/L, 15.0 mg/L, 30 mg/L, 60 mg/L, 120 mg/L, 250 mg/L, 500 mg/L silica standard solutions. 1-5 mL of various silica standard solutions were added to solid reagent A, shaken well, and then solid reagent B was added, shaken well, and the color was basically stable after 1-5 minutes of color development. The results are shown in Figure 4. It shows that without adding a masking agent, the kit cannot eliminate the interference of elements such as silicon.
  • This embodiment provides a detection kit, the raw materials of each component of reagent A are: 7g aminosulfonic acid, 1g sodium molybdate, and 2g sodium chloride.
  • the raw materials of each component of reagent B are: 5g aminosulfonic acid, 0.2g potassium antimony tartrate, and 4g sodium chloride.
  • Reagent A and reagent B are prepared according to the above method, and reagent A and reagent B are evenly packaged into 0.2g per tube.
  • silica stock solution 1000 mg/L to prepare silica standard solutions with concentrations of 0.02 mg/L, 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, 0.4 mg/L, 0.8 mg/L, 1.5 mg/L, 3.0 mg/L, 6.0 mg/L, 12.0 mg/L, 25 mg/L, and 50 mg/L.
  • Add 1-5 mL of various silica standard solutions add solid reagent B respectively, shake well, and then add solid reagent A. Add the masking agent, shake well, and the color will be basically stable after 1-5 minutes of color development.
  • Figure 5 This shows that without adding the masking agent, the kit cannot eliminate the interference of elements such as silicon.
  • the results are shown in Figure 5. Changing the order of adding the reagents cannot eliminate the interference of elements such as silicon.

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Abstract

一种磷酸根的检测试剂、检测试剂盒和检测方法。检测试剂包括试剂A和试剂B，试剂A包括强酸性试剂、钼酸盐和增重剂，其中强酸性试剂、钼酸盐和增重剂的质量比为(2～98)：(0.2～20.0)：(0～50.0)，试剂B包括强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂，其中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(2～98)：(1.0～30.0)：(0.5～50.0)：(0.1～50.0)：(0～50.0)。检测试剂无特殊环境要求，无特殊三废污染，成本低廉，检测步骤简单无干扰且测定更为准确，显色时间短且可移动性强。

Description

一种磷酸根的检测试剂、检测试剂盒和检测方法 技术领域
本发明属于分析化学技术领域，具体涉及一种磷酸根的检测试剂、检测试剂盒和检测方法。
背景技术
磷是生物生长必需的元素之一，但水体中磷含量过高会干扰水厂中的混凝过程。磷是藻类生长需要的一种关键元素，磷含量过多会引起藻类植物的过度生长，会使水质富营养化，影响水体生态平衡。一般天然水中磷酸盐含量不高，其主要来源为生活污水、化肥、冶炼、有机磷农药及合成洗涤剂等行业的工业废水。磷是评价水质的重要指标之一。
目前磷酸盐的测定常用重量法、滴定法、离子色谱法、分光光度法、原子吸收分光光度法、拉曼光谱法等。其中分光光度法是最常用的方法，在水质检测行业应用的比较多，其优点是简单、快捷、准确，而且已经有了完备的标准分析测定方法，但该法试剂用量大，环境污染重，繁琐费时，专业要求高，应急困难，限制了其在快速检测中的应用。重量法的优点是具有较高的准确度，至今仍被国内外作为标准方法推荐，适用于标准实验室和研究机构，但其缺点是分析速度慢，所以不可能用于企业现场分析。滴定法的优点是可非常准确测试磷含量，区别于仪器分析的办法，因为磷含量比较高超出测定范围，需要多次吸收进行检测引起实验误差，其缺点是比较繁琐，为传统的化学法滴定，耗时耗力，不符合现在科技需求。快速测试包法的优点是便宜，只需要几百块就可以检测几十次，快速，只需要5分钟可以出结果，且轻巧方便，其缺点是准确度不够，只可估算一个大范围值。
现有检测水系中磷酸盐含量常用钼酸铵分光光度法，该方法包括钼黄法或钼蓝法，酸铵分光光度法操作简单、花费少。钼黄法是磷酸与钒酸、钼酸作用形成磷钒钼黄杂多酸直接测定。但是，在现有的钼黄法中，一般使用的是硫酸或硝酸之类强酸的液态溶液。而该强酸的液体溶液对运输的要求高，操作繁琐，不安全，有一定的危险性。钼蓝法是将活性磷酸盐与钼酸盐反应生成磷钼黄，用还原剂将磷钼黄还原为磷钼蓝，其颜色深浅与有效磷的浓度成正比，在一定范围内符合朗伯比尔定律，从而可以用比色法进行测定。所用还原剂有氯化亚锡、抗坏血酸、硫酸联胺和亚硫酸盐等。但是存在以下不足，需要特定的设备成本较高、操作繁琐、专业要求高、应急困难等，限制了其在快速检测中的应用。为了弥补上述检测的短板， 近年来开发了快速、准确、携带方便、操作简单、快捷的磷酸根检测试剂盒。但在实际操作中，发现这些试剂盒一般假阳性比较高，没法消除砷、硅等元素的干扰。
公开号为CN106442511A的中国专利公开了一种磷酸盐快速检测试剂盒及检测方法，利用该检测试剂盒及其配套试纸的检测方法，可以使得磷酸盐的整个检测过程只需要2min，过程大大简化，保质期可达两年。但缺点在于无法消除砷、硅等元素的干扰。另外使用的是硫酸或硝酸之类强酸的液态溶液。而该强酸的液体溶液对运输的要求高，操作繁琐，不安全，有一定的危险性。
因此提高试剂盒测量灵敏度并消除其他元素的干扰是目前需要解决的一个关键问题。
发明内容
本发明的目的是为了克服现有技术存在的缺点和不足，而提供一种磷酸根的检测试剂、检测试剂盒和检测方法。
本发明具体技术方案如下：
本发明一方面提供一种磷酸根的检测试剂，所述检测试剂包括试剂A和试剂B；
所述试剂A包括强酸性试剂、钼酸盐和增重剂，其中强酸性试剂、钼酸盐和增重剂的质量比为(2～98)：(0.2～20.0)：(0～50.0)；
所述试剂B包括强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂，其中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(2～98)：(1.0～30.0)：(0.5～50.0)：(0.1～50.0)：(0～50.0)。
进一步地，所述试剂A中强酸性试剂、钼酸盐和增重剂的质量比为(5～10)：(0.5～2.0)：(0～5.0)；
所述试剂B中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(5～10)：(1.0～5.0)：(0.5～1.5)：(0.1～0.5)：(0～5.0)。
优选地，所述试剂A中强酸性试剂、钼酸盐和增重剂的质量比为7：1：2；
所述试剂B中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为5：1：1：0.2：2。
进一步地，所述强酸性试剂选自氨基磺酸、柠檬酸、羟基乙酸中的一种或以上；
所述钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或以上；
所述掩蔽剂包括酒石酸钾钠、柠檬酸、草酸、酒石酸、EDTA中的一种或以上；
所述还原剂包括抗坏血酸、硫酸肼、二氯化锡、氯化钠-氯化亚锡、硫酸联氨、1-氨基-2-荼酚-4-磺酸、硫酸合对甲氨基酚、对苯二酚、苯氨基硫脲、硫酸亚铁铵-果糖、硫酸亚铁铵-葡萄糖、焦亚硫酸钠、米吐尔、甲醛次亚硫酸氢钠、三氯化钛、亚硫酸盐-铁盐、硫酸亚铁铵、亚硫酸钠、亚硫酸氢钠以及锑(III)中的至少一种；
所述增速剂为酒石酸锑钾、硝酸铋中的至少一种；
所述增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或以上。
进一步地，所述强酸性试剂为氨基磺酸，所述钼酸盐为钼酸钠，所述掩蔽剂为酒石酸钾钠，所述还原剂为抗坏血酸，所述增速剂为酒石酸锑钾，所述增重剂为氯化钠。
本发明另一方面提供一种磷酸根的检测试剂盒，所述试剂盒包括试剂A和试剂B，以及标准比色卡。
本发明另一方面提供上述检测试剂盒的制备方法，包括步骤：
制备试剂A：按照上述的质量比将强酸性试剂、钼酸盐和增重剂充分研磨，研磨后的混合组分能通过80目标准筛，分装后，进行抽真空或通惰性气体密封；
制备试剂B：按照上述的质量比将强酸性试剂、掩蔽剂、还原剂、增重剂和增速剂充分研磨，研磨后的混合组分能通过80目标准筛，分装后，进行抽真空或通惰性气体密封；
制备标准比色卡：配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L磷酸根标准溶液，取各种磷酸根标准液1-5mL，分别加入所述的试剂A，摇匀，然后加入试剂B，摇匀，显色1-5min后，制得标准比色卡。
进一步地，试剂A和试剂B分装成每管0.1-0.5g。
本发明另一方面还提供一种磷酸根的检测方法，采用所述的检测试剂盒进行检测，包括步骤：将1-5mL待测水样加入至试剂A中，摇匀，然后加入试剂B，摇匀，1-5min后，与标准比色卡进行比对，确定待测水样中磷酸根的浓度。
本发明检测试剂盒应保存在阴凉干燥处，保存温度最好低于26℃。若温度高于25℃，则应把未用过的试纸袋放到冰箱中的保鲜层中保存，并放入避光防潮的包装中保存。本发明检测试剂盒的有效使用期为一年左右。
本发明的有益效果为：
1、本发明磷酸根检测方法基于磷钼蓝法，是一种不需要仪器设备、生产及使用成本低的快速灵活的磷酸根快速检测方法。本发明试剂盒无特殊环境要求，无特殊三废污染，成本低廉，检测步骤简单无干扰且测定更为准确，显色时间短且可移动性强。本发明与传统方法或 其他测定形式相比，使用更便捷，不需要专门技术人员进行测定。本发明所使用试剂都是普通的化学试剂，安全可靠，价格低廉。应用范围广，可用于测定化工污水、地表水、城市污水再生利用-景观环境用水以及城市杂用水等水体的磷酸根含量，尤其是环保领域磷酸根的监测中。
2、本发明通过在试剂A加入较多的酸，从而消除砷、硅等元素的干扰。待测水样中磷酸盐与试剂A中的钼酸盐反应，生成淡黄色的磷钼黄，然后加入的试剂B中的掩蔽剂可以螯合钼酸盐中的钼，从而提高检测灵敏度。
附图说明
图1为实施例1检测试剂盒的标准比色卡。
图2为实施例1的显色结果；
图3为实施例2的显色结果；
图4为实施例3的显色结果；
图5为实施例4的显色结果。
具体实施方式
为了更清楚地理解本发明，现参照下列实施例及附图进一步描述本发明。实施例仅用于解释而不以任何方式限制本发明。实施例中，各原始试剂材料均可商购获得，未注明具体条件的实验方法为所属领域熟知的常规方法和常规条件，或按照仪器制造商所建议的条件。
本实施例提供一种磷酸根的检测试剂盒，该试剂盒包括试剂A、试剂B和标准比色卡，具体制备方法如下：
试剂A的制备：按照强酸性试剂、钼酸盐和增重剂的质量比为(2～98)：(0.2～20.0)：(0～50.0)，准备强酸性试剂、钼酸盐、增重剂，将上述组分加入到研钵中，充分研磨至全部原材料均能通过80目标准筛，然后分装成每管0.1-0.5克，进行抽真空或通惰性气体密封。在一个优选的实施方案中，强酸性试剂、钼酸盐和增重剂的质量比为(5～10)：(0.5～2.0)：(0～5.0)。
试剂B的制备：按照强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(2～98)：(1.0～30.0)：(0.5～50.0)：(0.1～50.0)：(0～50.0)，准备强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂，将上述组分加入到研钵中，充分研磨至全部原材料均能通过80目标准筛，然后分装成每管0.1-0.5克，进行抽真空或通惰性气体密封。在一个优选的实施方案中，强酸性试 剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(5～10)：(1.0～5.0)：(0.5～1.5)：(0.1～0.5)：(0～5.0)。
标准比色卡制备：采用磷酸根储备液(1000mg/L)配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L磷酸根标准溶液，取各种磷酸根标准液1-5mL，分别加入A固体试剂，摇匀，然后加入B固体试剂，摇匀，显色1-5分钟后颜色基本稳定，制得标准比色卡。
其中，强酸性试剂选自氨基磺酸、柠檬酸、羟基乙酸中的一种或以上；
钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或以上；
掩蔽剂包括酒石酸钾钠、柠檬酸、草酸、酒石酸、EDTA中的一种或以上，掩蔽剂用于螯合钼酸盐中的钼；
还原剂包括抗坏血酸、硫酸肼、二氯化锡、氯化钠-氯化亚锡、硫酸联氨、1-氨基-2-荼酚-4-磺酸、硫酸合对甲氨基酚、对苯二酚、苯氨基硫脲、硫酸亚铁铵-果糖、硫酸亚铁铵-葡萄糖、焦亚硫酸钠、米吐尔、甲醛次亚硫酸氢钠、三氯化钛、亚硫酸盐-铁盐、硫酸亚铁铵、亚硫酸钠、亚硫酸氢钠以及锑(III)中的至少一种；
增速剂为酒石酸锑钾、硝酸铋中的至少一种；
增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或以上，增重剂便于试剂A和试剂B的称量。
制备的检测试剂盒应保存在阴凉干燥处，保存温度最好低于26℃。若温度高于25℃，则应把未用过的试纸袋放到冰箱中的保鲜层中保存，并放入避光防潮的包装中保存。
本实施例进一步提供一种磷酸根的检测方法，采用制备的检测试剂盒进行检测，包括步骤：将1-5mL待测水样加入至试剂A中，摇匀，然后加入试剂B，摇匀，1-5min后，如果水中存在磷酸根则显示蓝绿色，颜色的深浅与水中磷酸根的浓度相关，与标准比色卡进行比对，确定待测水样中磷酸根的浓度。
实施例1
本实施例提供一种检测试剂盒，试剂A各组分原材料为：氨基磺酸7g，钼酸钠1g，氯化钠2g。试剂B各组分原材料为：氨基磺酸5g，酒石酸钾钠1g，抗坏血酸1g，酒石酸锑钾0.2g，氯化钠2g。按照上述方法制备试剂A和试剂B，试剂A和试剂B均分装成每管0.2g。
采用磷酸根储备液(1000mg/L)配制浓度为0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、30mg/L、50mg/L、100mg/L、200mg/L、500mg/L、 1000mg/L磷酸根标准溶液，取各种磷酸根标准液1-5mL，分别加入A固体试剂，摇匀，然后加入B固体试剂，摇匀，显色1-5分钟后颜色基本稳定，不同浓度磷酸根标准溶液的显色结果如图2所示，基于本实施例试剂盒基于该试剂A和试剂B所制备的标准比色卡如图1所示。
实施例2
本实施例提供一种检测试剂盒，试剂A各组分原材料为：氨基磺酸1g，钼酸钠1g，氯化钠8g。试剂B各组分原材料为：氨基磺酸1g，酒石酸钾钠1g，抗坏血酸1g，酒石酸锑钾0.2g，氯化钠7g。按照上述方法制备试剂A和试剂B，试剂A和试剂B均分装成每管0.2g。
采用二氧化硅储备液(1000mg/L)配制浓度为0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、30mg/L、50mg/L、100mg/L二氧化硅标准溶液，取各种二氧化硅标准液1-5mL，分别加入A固体试剂，摇匀，然后加入B固体试剂，摇匀，显色1-5分钟后颜色基本稳定。结果如图3所示。说明降低酸的浓度，该试剂盒无法排除硅等元素的干扰。
实施例3
本实施例提供一种检测试剂盒，试剂A各组分原材料为：氨基磺酸7g，钼酸钠1g，氯化钠2g。试剂B各组分原材料为：氨基磺酸5g，酒石酸锑钾0.2g，氯化钠4g。按照上述方法制备试剂A和试剂B，试剂A和试剂B均分装成每管0.2g。
采用二氧化硅储备液(1000mg/L)配制浓度为0.25mg/L、0.5mg/L、1.0mg/L、2.0mg/L、4.0mg/L、8.0mg/L、15.0mg/L、30mg/L、60mg/L、120mg/L、250mg/L、500mg/L二氧化硅标准溶液，取各种二氧化硅标准液1-5mL，分别加入A固体试剂，摇匀，然后加入B固体试剂，摇匀，显色1-5分钟后颜色基本稳定。结果如图4所示。说明不加隐蔽剂，该试剂盒无法排除硅等元素的干扰。
实施例4
本实施例提供一种检测试剂盒，试剂A各组分原材料为：氨基磺酸7g，钼酸钠1g，氯化钠2g。试剂B各组分原材料为：氨基磺酸5g，酒石酸锑钾0.2g，氯化钠4g。按照上述方法制备试剂A和试剂B，试剂A和试剂B均分装成每管0.2g。
采用二氧化硅储备液(1000mg/L)配制浓度为0.02mg/L、0.05mg/L、0.1mg/L、0.2mg/L、0.4mg/L、0.8mg/L、1.5mg/L、3.0mg/L、6.0mg/L、12.0mg/L、25mg/L、50mg/L二氧化硅标准溶液，取各种二氧化硅标准液1-5mL，分别加入B固体试剂，摇匀，然后加入A固体试 剂，摇匀，显色1-5分钟后颜色基本稳定。结果如图5所示。说明不加隐蔽剂，该试剂盒无法排除硅等元素的干扰。结果如图5所示。改变试剂的加样顺序，无法排除硅等元素的干扰。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (9)

  1. 一种磷酸根的检测试剂，其特征在于，所述检测试剂包括试剂A和试剂B；
    所述试剂A包括强酸性试剂、钼酸盐和增重剂，其中强酸性试剂、钼酸盐和增重剂的质量比为(2～98)：(0.2～20.0)：(0～50.0)；
    所述试剂B包括强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂，其中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(2～98)：(1.0～30.0)：(0.5～50.0)：(0.1～50.0)：(0～50.0)。
  2. 根据权利要求1所述的检测试剂，其特征在于，所述试剂A中强酸性试剂、钼酸盐和增重剂的质量比为(5～10)：(0.5～2.0)：(0～5.0)；
    所述试剂B中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为(5～10)：(1.0～5.0)：(0.5～1.5)：(0.1～0.5)：(0～5.0)。
  3. 根据权利要求1所述的检测试剂，其特征在于，所述试剂A中强酸性试剂、钼酸盐和增重剂的质量比为7：1：2；
    所述试剂B中强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂的质量比为5：1：1：0.2：2。
  4. 根据权利要求1-3任一项所述的检测试剂，其特征在于，所述强酸性试剂选自氨基磺酸、柠檬酸、羟基乙酸中的一种或以上；
    所述钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或以上；
    所述掩蔽剂包括酒石酸钾钠、柠檬酸、草酸、酒石酸、EDTA中的一种或以上；
    所述还原剂包括抗坏血酸、硫酸肼、二氯化锡、氯化钠-氯化亚锡、硫酸联氨、1-氨基-2-荼酚-4-磺酸、硫酸合对甲氨基酚、对苯二酚、苯氨基硫脲、硫酸亚铁铵-果糖、硫酸亚铁铵-葡萄糖、焦亚硫酸钠、米吐尔、甲醛次亚硫酸氢钠、三氯化钛、亚硫酸盐-铁盐、硫酸亚铁铵、亚硫酸钠、亚硫酸氢钠以及锑(III)中的至少一种；
    所述增速剂为酒石酸锑钾、硝酸铋中的至少一种；
    所述增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或以上。
  5. 根据权利要求1-3任一项所述的检测试剂，其特征在于，所述强酸性试剂为氨基磺酸，所述钼酸盐为钼酸钠，所述掩蔽剂为酒石酸钾钠，所述还原剂为抗坏血酸，所述增速剂为酒石酸锑钾，所述增重剂为氯化钠。
  6. 一种磷酸根的检测试剂盒，其特征在于，所述试剂盒包括权利要求1所述的试剂A和试剂B，以及标准比色卡。
  7. 权利要求6所述检测试剂盒的制备方法，其特征在于，包括步骤：
    制备试剂A：按照权利要求1所述的质量比将强酸性试剂、钼酸盐和增重剂充分研磨，研磨后的混合组分能通过80目标准筛，分装后，进行抽真空或通惰性气体密封；
    制备试剂B：按照权利要求1所述的质量比将强酸性试剂、掩蔽剂、还原剂、增速剂和增重剂充分研磨，研磨后的混合组分能通过80目标准筛，分装后，进行抽真空或通惰性气体密封；
    制备标准比色卡：配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L磷酸根标准溶液，取各种磷酸根标准液1-5mL，分别加入所述的试剂A，摇匀，然后加入试剂B，摇匀，显色1-5min后，制得标准比色卡。
  8. 根据权利要求7所述的制备方法，其特征在于，试剂A和试剂B分装成每管0.1-0.5g。
  9. 一种磷酸根的检测方法，其特征在于，采用权利要求6所述的检测试剂盒进行检测，包括步骤：将1-5mL待测水样加入至试剂A中，摇匀，然后加入试剂B，摇匀，1-5min后，与标准比色卡进行比对，确定待测水样中磷酸根的浓度。
PCT/CN2023/139465 2023-12-18 2023-12-18 一种磷酸根的检测试剂、检测试剂盒和检测方法 Pending WO2025129388A1 (zh)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4599316A (en) * 1983-12-02 1986-07-08 Hoffmann-La Roche Inc. Photometric method for the determination of inorganic phosphate in liquid samples
KR20130107069A (ko) * 2012-03-21 2013-10-01 국립대학법인 울산과학기술대학교 산학협력단 수질 분석장치, 및 이를 이용한 수질 분석방법
CN106442511A (zh) * 2016-11-21 2017-02-22 广东环凯微生物科技有限公司 一种水质磷酸盐快速检测试剂盒及检测方法
CN110168377A (zh) * 2016-11-10 2019-08-23 英国研究与创新组织 用于测量化学物种的钼蓝测定

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4599316A (en) * 1983-12-02 1986-07-08 Hoffmann-La Roche Inc. Photometric method for the determination of inorganic phosphate in liquid samples
KR20130107069A (ko) * 2012-03-21 2013-10-01 국립대학법인 울산과학기술대학교 산학협력단 수질 분석장치, 및 이를 이용한 수질 분석방법
CN110168377A (zh) * 2016-11-10 2019-08-23 英国研究与创新组织 用于测量化学物种的钼蓝测定
CN106442511A (zh) * 2016-11-21 2017-02-22 广东环凯微生物科技有限公司 一种水质磷酸盐快速检测试剂盒及检测方法

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