WO2025129393A1 - 一种硅酸根的检测试剂、检测试剂盒和检测方法 - Google Patents

一种硅酸根的检测试剂、检测试剂盒和检测方法 Download PDF

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WO2025129393A1
WO2025129393A1 PCT/CN2023/139509 CN2023139509W WO2025129393A1 WO 2025129393 A1 WO2025129393 A1 WO 2025129393A1 CN 2023139509 W CN2023139509 W CN 2023139509W WO 2025129393 A1 WO2025129393 A1 WO 2025129393A1
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reagent
acid
water
silicate
molybdate
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French (fr)
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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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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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • 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

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  • the invention belongs to the technical field of materials, and in particular relates to a detection reagent, a detection kit and a detection method for silicate.
  • the silicon content in water is also a commonly measured parameter of water quality. If the content is too high, it will not only increase the amount of scale generated, but also increase the hardness of the scale. When the silicon dioxide in the circulating cooling water exceeds the limit concentration, it will easily cause pipe blockage and even cause serious accidents. In order to prevent accidents, it is necessary to detect the silicon content in industrial water in real time. When the silicon content is too high, the industrial water needs to be desiliconized.
  • Gravimetric method generally includes secondary hydrochloric acid evaporation and dehydration method, primary hydrochloric acid evaporation and dehydration method, chlorination method, polyethylene oxide condensation gravimetric method and animal gel condensation gravimetric method.
  • Titration method is commonly used in the determination of silicon dioxide in cement, metallurgy, new inorganic materials, glass products and their raw materials.
  • Spectrophotometry is widely used in the water quality testing industry. Silicon and phosphate react with molybdate in an acidic environment to generate yellow silico-molybdenum heteropolyacid complexes and group heteropolyacid complexes.
  • citric acid can destroy the phosphorus-containing complexes, leaving only yellow silicon-containing compounds for quantitative determination.
  • the silicon content is high, the yellow color left is darker, and its color depth is proportional to the concentration of effective silicon. It conforms to Lambert-Beer's law within a certain range, so it can be determined by colorimetry.
  • this detection method requires specific equipment, high cost, cumbersome operation, high professional requirements, and emergency difficulties, which limits its application in rapid detection.
  • a rapid, accurate, easy-to-carry, simple-to-operate and quick silicate detection kit has been developed in recent years.
  • silicate detection kits are all based on the reaction principle of silicomolybdenum yellow or silicomolybdenum blue.
  • silicic acid and ammonium molybdate generate yellow silicomolybdenum heteropoly acid (silicomolybdenum yellow method)
  • mask phosphorus with oxalic acid and reduce it to silicomolybdenum blue complex (silicomolybdenum blue method) with ascorbic acid, and its color depth is proportional to the concentration of effective silicon, and conforms to Lambert-Beer's law within a certain range, so that it can be measured by colorimetry.
  • test kits In actual operation, it is found that these test kits generally have high false positives, and the interference of elements such as arsenic and phosphorus cannot be eliminated. Therefore, improving the measurement sensitivity of the test kit and eliminating the interference of other elements is a key problem that needs to be solved at present.
  • the silicate detection kits or silicate detection test strips currently available in the market all require multi-step operation, are not suitable for field operations, and the reagent storage period is short, and it is not easy to preserve for a long time. Therefore, it is urgent to improve the assay method of existing silicate.
  • the Chinese patent with publication number CN115931757A provides a reagent combination for determining silicate, a preparation method thereof, and a method for determining silicate, which can determine silicate using non-hazardous raw materials, thereby reducing the reagent cost for determining silicate and increasing the safety of experimenters.
  • 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 chromaticity and reducing substances in high-interference wastewaters such as domestic sewage, landfill leachate or sewage with excessive concentration that can be diluted by setting acidification steps, oxidation steps and color development steps.
  • these are pre-treatment steps for sewage, and do not improve the molybdenum blue color development method, nor can they eliminate the interference of elements such as arsenic and phosphorus.
  • the purpose of the present invention is to overcome the shortcomings and deficiencies of the prior art and to provide a detection reagent, a detection kit and a detection method for silicate.
  • the present invention provides a silicate detection reagent, the detection reagent comprising reagent 1, reagent 2 and reagent 3;
  • the reagent 1 comprises a strong acidic reagent and a weighting agent, and the mass ratio of the strong acidic reagent to the weighting agent is (1-10):(2-10);
  • the reagent 2 includes molybdate and water, and the mass volume ratio (g:mL) of the molybdate to water is (1-50):(1-50);
  • the reagent 3 includes a masking agent, a reducing agent and water, and the mass volume ratio (g:g:mL) of the masking agent, the reducing agent and the water is (2-30):(10-50):(1-100).
  • the strong acidic agent is selected from a mixture of one or more of sulfamic acid, citric acid, glycolic acid, benzenesulfonic acid, substituted benzenesulfonic acid, and trichloroacetic acid;
  • the molybdate includes one or more of sodium molybdate, ammonium molybdate and potassium molybdate;
  • the masking agent includes one or more of citric acid, oxalic acid, tartaric acid, and EDTA;
  • the reducing agent includes one or more of ferrous sulfate, ascorbic acid, and tin chloride;
  • the weighting agent includes one or more of sodium chloride, sodium sulfate and potassium sulfate.
  • substituent of the substituted benzenesulfonic acid is selected from C1-C4 alkyl, chlorine, bromine or iodine;
  • the substituted benzene sulfonic acid includes o-C1-C4 alkylbenzene sulfonic acid, m-C1-C4 alkylbenzene sulfonic acid, p-C1-C4 alkylbenzene sulfonic acid, o-chlorobenzene sulfonic acid, m-chlorobenzene sulfonic acid, p-chlorobenzene sulfonic acid, o-bromobenzene sulfonic acid, m-bromobenzene sulfonic acid, p-bromobenzene sulfonic acid;
  • the substituted benzenesulfonic acid is selected from p-toluenesulfonic acid.
  • the strong acidic agent is selected from aminosulfonic 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.
  • Another aspect of the present invention provides a silicate detection kit, which comprises the above-mentioned detection reagent.
  • kit also includes 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 1 Grind the strong acid reagent and the weighting agent according to the ratio, and the mixed components after grinding can pass through an 80-mesh standard sieve. After packaging, vacuumize or seal with inert gas;
  • the reagent 1 is packaged into 0.1-0.5 g per tube.
  • the preparation method also includes the preparation of a standard colorimetric card: using a silicon dioxide stock solution to prepare a silicate standard solution with a concentration 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, taking 1 to 5 ml of various silicate standard solutions, adding them to the reagent 1 respectively, shaking well, then adding 1 to 5 drops of reagent 2, shaking well, then adding 1 to 5 drops of reagent 3, shaking well, and coloring for 1 to 5 minutes to obtain a standard colorimetric card.
  • the present invention also provides a method for detecting silicate, which adopts the above-mentioned detection kit for detection, comprising the steps of: adding 1 to 5 mL of a water sample to be tested into a reagent 1, shaking well, then adding 1 to 5 drops of a reagent 2, shaking well, then adding 1 to 5 drops of a reagent 3, shaking well, and after color development for 1 to 5 minutes, comparing with a standard colorimetric card to determine the concentration of silicate in the water sample to be tested.
  • the detection kit of the present invention is 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 silicate detection method of the present invention is based on the silicon molybdenum blue method. It is a fast and flexible silicate rapid detection method that does not require instruments and 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 without interference, more accurate determination, short color development time and strong mobility. Compared with traditional methods or other determination forms, the present invention is more convenient to use and does not require specialized technicians to perform determinations.
  • 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 silicate 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 environmental silicate.
  • the silicate detection kit of the present invention reduces the interference of phosphorus by controlling the acidity and reducing the amount of acid added. When used for silicate detection in water samples, it has strong anti-interference ability and a short detection time of only 5 minutes. The operation is simple, and the kit is small in size and can be carried around.
  • Fig. 1 is a standard colorimetric card for the detection kit of the present invention
  • 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 detection kit for silicate, which includes reagent 1, reagent 2, reagent 3 and a standard colorimetric card.
  • Reagent 1 includes 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);
  • reagent 2 includes molybdate and water, and the mass volume ratio of the molybdate to water (g: mL) is (1-50): (1-50);
  • reagent 3 includes a masking agent, a reducing agent and water, and the mass volume ratio of the masking agent, the reducing agent and water (g: g: mL) is (2-30): (10-50): (1-100).
  • the preparation method is as follows:
  • reagent 1 according to the ratio, the strong acid reagent and the weighting agent are fully ground, and the mixed components after grinding can pass through an 80-mesh standard sieve. After packaging, vacuum or inert gas is passed to seal; preferably, reagent 1 is packaged into 0.1-0.5g per tube;
  • Preparation of standard colorimetric card Use silica stock solution to prepare silicate standard solutions with concentrations 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. Take 1-5ml of various silicate standard solutions, add them to the reagent 1, shake well, then add 1-5 drops of reagent 2, shake well, then add 1-5 drops of reagent 3, shake well, and color for 1-5 minutes to prepare the standard colorimetric card. If silicate exists in the water, it will show blue-green color. The depth of color is related to the concentration of silicate in the water. Compare it with the standard colorimetric card to determine the concentration of silicate in the water sample to be tested.
  • the strong acidic reagent is selected from a mixture of one or more of aminosulfonic 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 benzenesulfonic acid includes o-C1-C4 alkylbenzenesulfonic acid, m-C1-C4 alkylbenzenesulfonic acid, p-C1-C4 alkylbenzenesulfonic acid, o-chlorobenzenesulfonic acid, m-chlorobenzenesulfonic acid, p-chlorobenzenesulfonic acid, o-bromobenzenesulfonic acid, m-bromobenzene,
  • the masking agent includes one or more of citric acid, oxalic acid, tartaric acid, and EDTA.
  • the reducing agent includes one or more of ferrous sulfate, ascorbic acid, and tin chloride.
  • the weighting agent includes one or more of sodium chloride, sodium sulfate, and potassium sulfate. The addition of the weighting agent facilitates the weighing of the powder.
  • This embodiment provides a silicate detection kit, which includes reagent 1, reagent 2, reagent 3 and a standard colorimetric card.
  • reagent 1 Add 2 g of aminosulfonic acid and 8 g of sodium chloride into a mortar and grind thoroughly until all raw materials can pass through an 80-mesh standard sieve. Then divide into 0.2 g tubes and evacuate or seal with inert gas.
  • silicate standard solutions with concentrations 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, and 1000mg/L.
  • reagent 1 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, and 1000mg/L.
  • the prepared standard colorimetric card is shown in FIG1 , and the color development result is shown in FIG2 .
  • This embodiment provides a detection kit, which includes reagent 1, reagent 2, and reagent 3.
  • reagent 1 Add 2 g of aminosulfonic acid and 8 g of sodium chloride into a mortar and grind thoroughly until all raw materials can pass through an 80-mesh standard sieve. Then divide into 0.2 g tubes and evacuate or seal with inert gas.
  • This embodiment provides a detection kit, which includes reagent 1, reagent 2, and reagent 3.
  • reagent 1 Add 2 g of aminosulfonic acid and 8 g of sodium chloride into a mortar and grind thoroughly until all raw materials can pass through an 80-mesh standard sieve. Then divide into 0.2 g tubes and evacuate or seal with inert gas.
  • phosphate standard solutions with 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, 50 mg/L, 100 mg/L, 200 mg/L, and 500 mg/L.
  • 1 to 5 ml of various phosphate standard solutions were added to the reagent 1, shaken, and then 1 to 5 drops of reagent 3 were added, shaken, and then 1 to 5 drops of reagent 2 were added, shaken, and color was developed for 1 to 5 minutes. The results are shown in Figure 4. Changing the order of adding the reagents cannot eliminate the interference of elements such as phosphorus.
  • This embodiment provides a detection kit, which includes reagent 1, reagent 2, and reagent 3.
  • silica stock solution was used to prepare silicate standard solutions of different concentrations, 1-5 ml of various silicate standard solutions were taken, and added to the reagent 1, shaken, and then 1-5 drops of reagent 2 were added, shaken, and then 1-5 drops of reagent 3 were added, shaken, and color was developed for 1-5 minutes.
  • the results are shown in Figure 5. It shows that other acids can also meet the requirements, but sulfuric acid, hydrochloric acid, etc. are liquid acids, which are relatively corrosive and difficult to transport, so liquid acids are not selected in the present invention.

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Abstract

一种硅酸根的检测试剂、检测试剂盒和检测方法；检测试剂包括试剂1、试剂2和试剂3；试剂1包括强酸性试剂和增重剂，强酸性试剂与增重剂的质量比为(1～10):(2～10)；试剂2包括钼酸盐和水，钼酸盐与水的质量体积比(g：mL)为(1～50):(1～50)；试剂3包括掩蔽剂、还原剂和水，掩蔽剂、还原剂与水质量体积比(g：g：mL)为(2～30):(10～50):(1～100)。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

一种硅酸根的检测试剂、检测试剂盒和检测方法 技术领域
本发明属于材料技术领域，具体涉及一种硅酸根的检测试剂、检测试剂盒和检测方法。
背景技术
几乎所有的工业生产过程都要用水，水质好坏对生产过程或产品有不同的影响。水中硅含量也是水质常测参数，其含量过高不仅增加水垢的生成量而且增加水垢的硬度。循环冷却水中的二氧化硅超出限定浓度后，也会容易导致管道堵塞，甚至造成严重事故。为了防止事故的出现，需要实时对工业用水中的硅含量进行检测，硅含量过高时需要对工业用水进行除硅处理。
硅酸根的检测方法也有很多，如重量法、滴定法以及分光光度法。重量法一般包括二次盐酸蒸干脱水法、一次盐酸蒸干脱水法、氯化法、聚环氧乙烷凝聚重量法、动物胶凝聚重量法。滴定法常用于广泛应用于水泥、冶金、新型无机材料、玻璃制品及其原料中二氧化硅的测定。分光光度法在水质检测行业应用的比较多，硅和磷酸盐在酸性环境下与钼酸盐反应，生成黄色的硅钼杂多酸配合物和组杂多酸配合物，柠檬酸等的加入可以破坏含磷配合物，而只留下显黄色的含硅化合物以定量测定。含硅量高时，留下的黄色就较深，其颜色深度与有效硅的浓度成正比，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。但是该检测方法需要特定的设备、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、快捷的硅酸根检测试剂盒。
现有的硅酸根检测试剂盒都是基于硅钼黄或硅钼蓝的反应原理。在酸性溶液中，硅酸与钼酸铵生成黄色的硅钼杂多酸(硅钼黄法)，然后以草酸掩蔽磷，用抗坏血酸将其还原为硅钼蓝络合物(硅钼蓝法)，其颜色深度与有效硅的浓度成正比，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。但在实际操作中，发现这些试剂盒一般假阳性比较高，无法消除砷、磷等元素的干扰。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。并且，目前市售的硅酸根检测试剂盒或硅酸根检测试纸均需要多步操作，不适用野外作业，试剂储存期短，不易长期保存。因此，急需改进现有硅酸根的测定方法。
公开号为CN115931757A的中国专利提供了一种用于测定硅酸根的试剂组合及其制备方法、测定硅酸根的方法，使用无危险的原料即可对硅酸根进行测定，降低了测定硅酸根的试剂成本以及增加实验人员安全性。但缺点在于无法消除砷、磷等元素的干扰。
公开号为CN114371165A的中国专利通过设置酸化步骤、氧化步骤和显色步骤，屏蔽了生活污水、垃圾渗滤液或者浓度过高可稀释后的污水等高干扰废水中较高的色度和还原性物质的干扰，但这些都是污水的前处理步骤，对钼蓝显色法并没有改进，也无法消除砷、磷等元素的干扰。
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，而提供一种硅酸根的检测试剂、检测试剂盒和检测方法。
本发明一方面提供一种硅酸根的检测试剂，所述检测试剂包括试剂1、试剂2和试剂3；
所述试剂1包括强酸性试剂和增重剂，所述强酸性试剂与增重剂的质量比为(1～10):(2～10)；
所述试剂2包括钼酸盐和水，所述钼酸盐与水的质量体积比(g：mL)为(1～50):(1～50)；
所述试剂3包括掩蔽剂、还原剂和水，所述掩蔽剂、还原剂与水质量体积比(g：g：mL)为(2～30):(10～50):(1～100)。
进一步地，所述强酸性试剂选自氨基磺酸、柠檬酸、羟基乙酸、苯磺酸、取代苯磺酸、三氯乙酸中的一种或多种的混合物；
所述钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或多种；
所述掩蔽剂包括柠檬酸、草酸、酒石酸、EDTA中的一种或多种；
所述还原剂包括硫酸亚铁、抗坏血酸、氯化锡中的一种或多种；
所述增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或多种。
进一步地，所述取代苯磺酸的取代基选自C1～C4烷基、氯、溴或碘；
优选地，所述取代苯磺酸包括邻C1～C4烷基苯磺酸、间C1～C4烷基苯磺酸、对C1～C4烷基苯磺酸、邻氯代苯磺酸、间氯代苯磺酸、对氯代苯磺酸、邻溴代苯磺酸、间溴代苯磺酸、对溴代苯磺酸；
优选地，所述取代苯磺酸选自对甲苯磺酸。
进一步地，所述强酸性试剂选自氨基磺酸；
所述钼酸盐选自钼酸铵；
所述掩蔽剂选自草酸；
所述还原剂选自抗坏血酸；
所述增重剂选自氯化钠。
本发明另一方面提供一种硅酸根的检测试剂盒，所述试剂盒包括上述的检测试剂。
进一步地，所述试剂盒还包括标准比色卡。
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1：按照配比，将强酸性试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；
制备试剂2：按照配比，将钼酸盐溶于水中；
制备试剂3：按照配比，将掩蔽剂和还原剂溶于水中。
进一步地，所述试剂1分装成每管0.1～0.5g。
进一步地，所述制备方法还包括标准比色卡的制备：采用二氧化硅储备液配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L硅酸根标准溶液，取各种硅酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，制得标准比色卡。
本发明还提供一种硅酸根的检测方法，采取上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1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，与标准比色卡进行比对，确定待测水样中硅酸根的浓度。
本发明检测试剂盒保存在阴凉干燥处，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、本发明硅酸根检测方法基于硅钼蓝法，是一种不需要仪器设备、生产及使用成本低的快速灵活的硅酸根快速检测方法。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硅酸根含量，尤其是环保硅酸根的监测中。
2、本发明硅酸根检测试剂盒通过控制酸度，减少酸的投量，以减小磷的干扰，在用于水样中硅酸根检测时抗干扰能力强，检测时间短，只需5分钟即可完成，操作简单，并且试剂盒体积小，可随身携带。
附图说明
图1为本发明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。
本实施例提供一种硅酸根的检测试剂盒，其包括试剂1、试剂2、试剂3和标准比色卡，试剂1包括强酸性试剂和增重剂，所述强酸性试剂与增重剂的质量比为(1～10):(2～10)；试剂2包括钼酸盐和水，所述钼酸盐与水的质量体积比(g：mL)为(1～50):(1～50)；试剂3包括掩蔽剂、还原剂和水，所述掩蔽剂、还原剂与水质量体积比(g：g：mL)为(2～30):(10～50):(1～100)。制备方法如下：
制备试剂1：按照配比，将强酸性试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；优选地，将试剂1分装成每管0.1～0.5g；
制备试剂2：按照配比，将钼酸盐溶于水中；
制备试剂3：按照配比，将掩蔽剂和还原剂溶于水中。
标准比色卡制备：采用二氧化硅储备液配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L硅酸根标准溶液，取各种硅酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，制得标准比色卡。如果水中存在硅酸根则显示蓝绿色，颜色的深浅与水中硅酸根的浓度相关，与标准比色卡进行比对，确定待测水样中硅酸根的浓度。
其中，强酸性试剂选自氨基磺酸、柠檬酸、羟基乙酸、苯磺酸、取代苯磺酸、三氯乙酸中的一种或多种的混合物；优选地，所述取代苯磺酸的取代基选自C1～C4烷基、氯、溴或碘；优选地，所述取代苯磺酸包括邻C1～C4烷基苯磺酸、间C1～C4烷基苯磺酸、对C1～C4烷基苯磺酸、邻氯代苯磺酸、间氯代苯磺酸、对氯代苯磺酸、邻溴代苯磺酸、间溴代苯磺酸、对溴代苯磺酸；优选地，所述取代苯磺酸选自对甲苯磺酸。
钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或多种。
掩蔽剂包括柠檬酸、草酸、酒石酸、EDTA中的一种或多种。
还原剂包括硫酸亚铁、抗坏血酸、氯化锡中的一种或多种。
增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或多种，增重剂的添加方便粉末的称取。
实施例1
本实施例提供一种硅酸根的检测试剂盒，其包括试剂1、试剂2、试剂3和标准比色卡。
制备试剂1：将氨基磺酸2g，氯化钠8g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0.2g，进行抽真空或通惰性气体密封。
制备试剂2：将钼酸铵0.5g溶于5mL水中。
制备试剂3：将草酸1g，抗坏血酸4g溶于10mL水中。
采用二氧化硅储备液配制浓度为0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L硅酸根标准溶液，取各种硅酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，制得标准比色卡。如果水中存在硅酸根则显示蓝绿色，颜色的深浅与水中硅酸根的浓度相关。
所制备的标准比色卡如图1所示，显色结果如图2所示。
实施例2
本实施例提供一种检测试剂盒，其包括试剂1、试剂2、试剂3。
制备试剂1：将氨基磺酸2g，氯化钠8g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0.2g，进行抽真空或通惰性气体密封。
制备试剂2：将钼酸铵0.5g溶于5mL水中。
制备试剂3：将抗坏血酸4g溶于10mL水中。
采用磷酸二氢钠储备液配制浓度为0mg/L、0.5mg/L、1mg/L、2mg/L、4mg/L、8mg/L、15mg/L、30mg/L、60mg/L、120mg/L、250mg/L磷酸根标准溶液，取各种磷酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3， 摇匀，显色1～5min后，结果如图3所示。说明不加隐蔽剂，该试剂盒无法排除磷等元素的干扰。
实施例3
本实施例提供一种检测试剂盒，其包括试剂1、试剂2、试剂3。
制备试剂1：将氨基磺酸2g，氯化钠8g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0.2g，进行抽真空或通惰性气体密封。
制备试剂2：将钼酸铵0.5g溶于5mL水中。
制备试剂3：将草酸1g，抗坏血酸4g溶于10mL水中。
采用磷酸二氢钠储备液配制浓度为0mg/L、0.1mg/L、0.2mg/L、0.5mg/L、1mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L磷酸根标准溶液，取各种磷酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂3，摇匀，然后加入1～5滴试剂2，摇匀，显色1～5min后，结果如图4所示。改变试剂的加样顺序，无法排除磷等元素的干扰。
实施例4
本实施例提供一种检测试剂盒，其包括试剂1、试剂2、试剂3。
制备试剂1：每管中加入0.1M的盐酸溶液。
制备试剂2：将钼酸铵0.5g溶于5mL水中。
制备试剂3：将草酸1g，抗坏血酸4g溶于10mL水中。
检测：采用二氧化硅储备液配制不同浓度的硅酸根标准溶液，取各种硅酸根标准液1～5ml，分别加入至所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，结果如图5所示。说明其他酸也能满足要求，但硫酸、盐酸等是液体酸，腐蚀性比较强，不易运输，所以本发明没有选择液体酸。
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 (11)

  1. 一种硅酸根的检测试剂，其特征在于，所述检测试剂包括试剂1、试剂2和试剂3；
    所述试剂1包括强酸性试剂和增重剂，所述强酸性试剂与增重剂的质量比为(1～10):(2～10)；
    所述试剂2包括钼酸盐和水，所述钼酸盐与水的质量体积比(g：mL)为(1～50):(1～50)；
    所述试剂3包括掩蔽剂、还原剂和水，所述掩蔽剂、还原剂与水质量体积比(g：g：mL)为(2～30):(10～50):(1～100)。
  2. 根据权利要求1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、苯磺酸、取代苯磺酸、三氯乙酸中的一种或多种的混合物；
    所述钼酸盐包括钼酸钠、钼酸铵、钼酸钾中的一种或多种；
    所述掩蔽剂包括柠檬酸、草酸、酒石酸、EDTA中的一种或多种；
    所述还原剂包括硫酸亚铁、抗坏血酸、氯化锡中的一种或多种；
    所述增重剂包括氯化钠、硫酸钠、硫酸钾中的一种或多种。
  3. 根据权利要求2所述的检测试剂，其特征在于，所述取代苯磺酸的取代基选自C1～C4烷基、氯、溴或碘。
  4. 根据权利要求2所述的检测试剂，其特征在于，所述取代苯磺酸包括邻C1～C4烷基苯磺酸、间C1～C4烷基苯磺酸、对C1～C4烷基苯磺酸、邻氯代苯磺酸、间氯代苯磺酸、对氯代苯磺酸、邻溴代苯磺酸、间溴代苯磺酸、对溴代苯磺酸；
    所述取代苯磺酸选自对甲苯磺酸。
  5. 根据权利要求1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；
    所述钼酸盐选自钼酸铵；
    所述掩蔽剂选自草酸；
    所述还原剂选自抗坏血酸；
    所述增重剂选自氯化钠。
  6. 一种硅酸根的检测试剂盒，其特征在于，所述试剂盒包括权利要求1所述的检测试剂。
  7. 根据权利要求6所述的检测试剂盒，其特征在于，所述试剂盒还包括标准比色卡。
  8. 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1：按照权利要求1所述配比，将强酸性试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；
    制备试剂2：按照权利要求1所述配比，将钼酸盐溶于水中；
    制备试剂3：按照权利要求1所述配比，将掩蔽剂和还原剂溶于水中。
  9. 根据权利要求8所述的制备方法，其特征在于，所述试剂1分装成每管0.1～0.5g。
  10. 根据权利要求8所述的制备方法，其特征在于，所述制备方法还包括标准比色卡的制备：采用二氧化硅储备液配制浓度为0mg/L、2.0mg/L、5.0mg/L、10.0mg/L、20mg/L、50mg/L、100mg/L、200mg/L、500mg/L、1000mg/L硅酸根标准溶液，取各种硅酸根标准液1～5ml，分别加入至权利要求7所述的试剂1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，制得标准比色卡。
  11. 一种硅酸根的检测方法，其特征在于，采取权利要求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1中，摇匀，然后加入1～5滴试剂2，摇匀，然后加入1～5滴试剂3，摇匀，显色1～5min后，与标准比色卡进行比对，确定待测水样中硅酸根的浓度。
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