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Detection reagent combination for determining phosphate molybdenum antimony resistance and preparation method thereof

A phosphate molybdenum antimony and detection reagent technology, applied in the field of chemical analysis, can solve problems such as easy decomposition and deterioration, ammonia nitrogen measurement error, inability to store for a long time, etc., and achieve the effects of eliminating interference, delaying decomposition and improving accuracy

Inactive Publication Date: 2020-06-05
SHENZHEN LIGHTSUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since this method is a manual colorimetric method, when it is applied to an online multi-parameter testing instrument, there are the following problems: First, the online multi-parameter nutrient detector usually measures other parameters such as ammonia nitrogen, nitrate, and nitrite at the same time. , and the ammonium molybdate reagent of phosphate itself will introduce interfering substances - ammonium ions (NH4+), if the instrument cannot be cleaned, it will easily cause errors in the determination of ammonia nitrogen; It is easy to decompose and deteriorate when exposed to light. When the instrument is working in the field, it cannot be stored for a long time

Method used

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  • Detection reagent combination for determining phosphate molybdenum antimony resistance and preparation method thereof
  • Detection reagent combination for determining phosphate molybdenum antimony resistance and preparation method thereof
  • Detection reagent combination for determining phosphate molybdenum antimony resistance and preparation method thereof

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preparation example Construction

[0023] The present invention also provides a method for preparing the detection reagent combination for the determination of the phosphate molybdenum antimony resistance method, which is used to prepare the above detection reagent combination, comprising the following steps:

[0024]Preparation mass fraction is the sodium molybdate of 8g / L-22g / L, the concentrated sulfuric acid that mass fraction is 72mL / L-93mL / L and the mass fraction is the antimony potassium tartrate of 80mL / L-150mL / L0.3%, take respectively A set amount of the sodium molybdate solution, the concentrated sulfuric acid and the antimony potassium tartrate are mixed and stirred evenly, and then the color reagent is obtained by constant volume with pure water; ascorbic acid with a mass fraction of 18g / L-32g / L is prepared , mass fraction of glacial acetic acid of 34mL-55mL / L and mass fraction of ethylenediaminetetraacetic acid tetrasodium salt of 0.5g / L-1.6g / L, respectively take set amount of said ascorbic acid, sai...

Embodiment 1

[0034] Control reagent combination:

[0035] Preparation of the national standard ammonium molybdate reagent: pipette 8.5mL of concentrated sulfuric acid, slowly add it to 70mL of pure water, and stir at the same time; after cooling to room temperature, weigh 0.6g of ammonium molybdate with a ten-thousandth balance and dissolve it in sulfuric acid , and add 10mL of 0.3% antimony potassium tartrate reagent, and set the volume to 100mL. Preparation of national standard ascorbic acid: Weigh 2g of ascorbic acid with a ten thousandth balance and dissolve in 100mL of pure water;

[0036] Experimental reagent combination (that is, the detection reagent combination of this application):

[0037] Preparation of color reagent: pipette 8.5mL of concentrated sulfuric acid into 70mL of pure water, cool to room temperature, weigh 1.2g of sodium molybdate dissolved in sulfuric acid with a ten-thousandth balance, and add 10mL of 0.3% antimony potassium tartrate solution, Add pure water to ma...

Embodiment 2

[0041] The control reagent combination and experimental reagent combination prepared in embodiment 1 were used to test,

[0042] At a concentration of 0.5mg / L PO 4 3- Under certain conditions, use two online instruments (μchem in-situ nutrient analyzer) to test in the laboratory; one is tested with the control reagent combination; the other is tested with the experimental reagent combination, running every 4 hours Once, run continuously for 15 days, the result is as follows image 3 shown. The national standard ascorbic acid in the control reagent combination began to gradually decline on the third day, and had dropped to 50% by the seventh day, and was completely ineffective on the tenth day; while the reducing reagent of the experimental reagent combination was not until the fifteenth day of operation, The test result is still within 0.5mg / L (±10%). It can be concluded that the stability and persistence of the reducing reagent of the experimental reagent combination are ...

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Abstract

The method is suitable for the technical field of chemical analysis, and discloses a detection reagent combination for determining phosphate molybdenum antimony resistance and a preparation method thereof. The detection reagent combination comprises a chromogenic reagent used for reacting with phosphate to generate phosphomolybdic heteropolyacid and a reducing reagent used for reducing phosphomolybdic heteropolyacid; the chromogenic reagent comprises sodium molybdate with the mass fraction being 8 g / L-22 g / L, concentrated sulfuric acid with the mass fraction being 72 mL / L-93 mL / L and antimonypotassium tartrate with the mass fraction being 80 mL / L-150 mL / L and the mass fraction being 0.3%. The reducing reagent comprises ascorbic acid with the mass fraction of 18 g / L-32 g / L, a weak acid solution with the mass fraction of 34 mL / L-55 mL / L and a decomposition inhibiting agent with the mass fraction of 0.5 g / L-1. 6 g / L. According to the detection reagent combination for determining phosphate molybdenum antimony resistance and the preparation method, the accuracy of phosphate content detection can be improved, and meanwhile, the expiration date of the reagent combination can be prolonged.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a detection reagent combination and a preparation method for the determination of phosphate molybdenum antimony resistance method. Background technique [0002] Phosphate is one of the important parameters for monitoring water quality. If the phosphate content in the water is too large, it will lead to eutrophication of the water quality. Eutrophication will affect the water quality of the water body, reduce the transparency of the water, and make it difficult for sunlight to penetrate. The permeable layer will affect the photosynthesis of plants in the water, and may cause the supersaturated state of dissolved oxygen, which is harmful to aquatic animals and causes a large number of fish deaths. The phosphate detection method used by mainstream online instruments is mainly molybdenum antimony anti-spectrophotometry. Under the strongly acidic condition of co...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N33/18
CPCG01N21/78G01N33/18G01N2021/775
Inventor 李固张全良谢佳裕高鸿杰魏剑达
Owner SHENZHEN LIGHTSUN TECH CO LTD