CN110646415A - Reagent for rapidly detecting magnesium hardness concentration in water and use method thereof - Google Patents

Reagent for rapidly detecting magnesium hardness concentration in water and use method thereof Download PDF

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Publication number
CN110646415A
CN110646415A CN201910922741.8A CN201910922741A CN110646415A CN 110646415 A CN110646415 A CN 110646415A CN 201910922741 A CN201910922741 A CN 201910922741A CN 110646415 A CN110646415 A CN 110646415A
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Prior art keywords
component
reagent
raw materials
magnesium
bag
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Inventor
李娟�
刘瑞杰
肖才斌
顾毅康
张旭
丁月培
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Changzhou Luopanxing Testing Technology Co Ltd
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Changzhou Luopanxing Testing Technology Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N2021/775Indicator and selective membrane

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention belongs to the technical field of environmental protection detection, and particularly relates to a reagent and a use method for rapidly detecting the hardness concentration of magnesium in water. The reagent for rapidly detecting the hardness concentration of the high-concentration magnesium in the water consists of A, B and C, wherein the weight ratio of A: b: c-2-3: 2-3: 1-2; the component A is a solid buffer reagent with the pH value of 9.5-11; the component B is a mixture of a buffer reagent and a masking agent reagent; the component C is a mixture of a filler and a calcium magnesium reagent-acid gran K. The detection reagent is a solid reagent bag, is convenient to carry and simple to use, has a quick test process, and can be matched with a portable Pyxis SP-910 multi-parameter water quality analyzer to quickly and accurately detect the high magnesium hardness content in industrial circulating water, surface water and sewage.

Description

Reagent for rapidly detecting magnesium hardness concentration in water and use method thereof
Technical Field
The invention belongs to the technical field of environmental protection detection, and particularly relates to a reagent and a use method for rapidly detecting the hardness concentration of magnesium in water.
Background
The magnesium ion concentration in water is the magnesium hardness, and when the magnesium ion concentration is too high, the magnesium ion concentration can react with carbonate, phosphate radical or silicate radical in water to generate magnesium carbonate, magnesium phosphate and magnesium silicate scale. The hardness of water is mainly calcium and magnesium, and the over-high hardness of water can cause harm to human health, daily life, industrial production and the like. For example, excessive magnesium sulfate in water can cause diarrhea. The measurement of magnesium hardness in water is carried out in many ways, but most of them are carried out in the laboratory, such as: with the development of modern analytical chemistry, limitations of a traditional water magnesium hardness analysis method on analysis efficiency and analysis capacity become more and more obvious, and application of the traditional water magnesium hardness analysis method in analysis of a complex water body system is limited. Reagents for testing magnesium hardness are mainly provided in the market by an EDTA titration method, a calcium-magnesium indicator method, an online titration method and the like. The reagent for measuring magnesium by the existing colorimetric method has low measuring range, only can measure a few ppm, and can only dilute dozens of times or even hundreds of times of harder water body for testing, so that the result can not accurately reflect the hardness of the water body.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defect of low reagent dosage range of rapid detection of magnesium hardness concentration in water in the prior art, and provides a reagent and a use method for rapid detection of high-concentration magnesium hardness concentration in water.
The invention realizes the purpose through the following technical scheme: a reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water comprises A, B and C, wherein the weight ratio of A: b: c-2-3: 2-3: 1-2;
the component A is a solid buffer reagent with the pH value of 9.5-11;
the component B is a mixture of a buffer reagent and a masking agent reagent;
the component C is a mixture of a filler and a calcium magnesium reagent-acid gran K.
Preferably, the component A is prepared from the following raw materials in parts by weight: adding 10g-20g of glycine, 2g-4g of lithium hydroxide, 0.1g-0.5g L-cysteine and 1g-5g of EDTA.4Na into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2-0.3g per bag to obtain a component A;
preferably, the component B is prepared from the following raw materials in parts by weight: adding 10g-20g of glycine, 2g-4g of lithium hydroxide, 0.1g-0.5g L-cysteine and 1g-5g of EGTA (ethylene glycol bis (2-aminoethyl ether) tetraacetic acid) into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2-0.3g of each package to obtain a component B;
preferably, the component C is prepared from the following raw materials in parts by weight: 5g to 15g of filler polyethylene glycol, 0.5g to 1.5g of calcium magnesium reagent and 0.5g to 1.5g of acid gran K, fully grinding the raw materials until all the raw materials are uniformly mixed, and then subpackaging into 0.1g to 0.2g of each bag to obtain the component C.
According to another aspect of the present invention, the present invention provides a method for using a reagent for rapidly detecting a high concentration of magnesium hardness in water, comprising the steps of:
when in use, two 10ml colorimetric bottles are taken, and water samples are respectively added to the scale marks; adding the component A into a colorimetric bottle, and shaking up to dissolve the component A to obtain a blank sample; adding the component B into another colorimetric bottle, and shaking up to dissolve the component B to obtain a sample to be detected; and adding two parts of the component C into two colorimetric bottles respectively, shaking uniformly for dissolving, reacting for 2min at a timing, putting a blank sample into a spectrophotometric analyzer after timing is finished, performing background calibration, and putting a sample to be detected into the spectrophotometric analyzer for reading.
The invention adopts the solid reagent package, avoids the frequent configuration and instability of the liquid reagent, greatly improves the reaction sensitivity in the buffer solution with the pH value of about 9.5-11, thereby ensuring the accuracy and the reproducibility of the result, and has the advantages of simple and convenient operation, accurate result, low price, convenient storage and transportation, suitability for on-site rapid detection and the like.
Compared with the prior art, the invention has the following advantages:
1) the invention adopts a spectrophotometry method to directly test the high-range magnesium hardness without dilution;
2) the method of the invention is convenient to operate, and the reagent and the detection instrument thereof are convenient to carry.
Drawings
FIG. 1 is a linear relationship diagram of the rapid detection reagent for magnesium hardness concentration of the present invention and different magnesium concentrations.
Detailed Description
In the embodiment of the invention, the ultraviolet spectrophotometer analyzer is replaced by a Pyxis SP-910 portable multi-parameter water quality analyzer.
Example 1
The reagent is packaged by A, B, C three components, and the specific manufacturing method comprises the following steps:
1. preparing raw materials of the component A according to the following proportion: adding 10g of glycine, 3g of lithium hydroxide, 0.1g L-cysteine and 1g of EDTA.4Na into a glass mortar, fully grinding the materials until all the raw materials are uniformly mixed, and then subpackaging into 0.2g of each bag to obtain a reagent A;
2. preparing raw materials for the component B according to the following proportion: 10g of glycine, 2g of lithium hydroxide, 0.1g of L-cysteine and 1g of EGTA, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2g of each bag to obtain a reagent B;
3. preparing raw materials for the component C according to the following proportion: 5g of polyethylene glycol 6000,0.5g of acid Glan K and 0.5g of calcium-magnesium reagent, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.1g of each bag to obtain the reagent C.
Example 2
The reagent is packaged by A, B, C three components, and the specific manufacturing method comprises the following steps:
1. preparing raw materials of the component A according to the following proportion: adding 15g of glycine, 3g of lithium hydroxide, 0.25g of 0.25g L-cysteine and 4.2g of EDTA.4Na into a glass mortar, fully grinding the materials until all the raw materials are uniformly mixed, and then subpackaging into 0.25g of each bag to obtain a reagent A;
2. preparing raw materials for the component B according to the following proportion: 15g of glycine, 3.2g of lithium hydroxide, 0.25g L-cysteine and 2.3g of EGTA, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.23 g of each bag to obtain a reagent B;
3. preparing raw materials for the component C according to the following proportion: 7.5g of polyethylene glycol 6000,1.2g of acid gran K and 1.2g of calcium-magnesium reagent, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.1g of each bag to obtain the reagent C.
Example 3
The reagent is packaged by A, B, C three components, and the specific manufacturing method comprises the following steps:
1. preparing raw materials of the component A according to the following proportion: adding 20g of glycine, 3g of lithium hydroxide, 0.5g L-cysteine and 5g of EDTA.4Na into a glass mortar, fully grinding the materials until all the raw materials are uniformly mixed, and then subpackaging into 0.3g of each bag to obtain a reagent A;
2. preparing raw materials for the component B according to the following proportion: 20g of glycine, 4g of lithium hydroxide, 0.5g of L-cysteine and 5g of EGTA, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.3g of each bag to obtain a reagent B;
3. preparing raw materials for the component C according to the following proportion: 15g of polyethylene glycol 8000,1.2g of acid Glan K and 1.2g of calcium-magnesium reagent, adding the materials into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2g of each bag to obtain the reagent C.
Example four
0.9521g of anhydrous magnesium chloride is precisely weighed, dissolved in water and fixed to 100ml, which is CaCO310000PPM of magnesium standard solution mother liquor is diluted to prepare a series of standard solutions with different concentrations, wherein the concentrations are respectively 10, 50, 100, 150 and 200 PPM. Two 10ml colorimetric bottles are taken, and water samples are respectively added to the scale marks. 1 part of reagent A (prepared in example 3)Adding one of the color comparison bottles, shaking up and dissolving to obtain a blank sample; adding 1 pack of reagent B (prepared in example 3) into another colorimetric bottle, and shaking up to dissolve the reagent B, wherein the reagent B is a sample to be detected; and then adding two bags of reagent C (prepared in example 3) into two colorimetric bottles respectively, shaking up for dissolving, timing for reaction for 2min, after timing is finished, putting a blank sample into an ultraviolet spectrophotometry analyzer for background calibration, and putting a sample to be detected into the spectrophotometry analyzer for reading. The linear relation is seen by taking the absorbance as the abscissa and the concentration as the ordinate, the linear relation between the hard magnesium concentration and the absorbance is good, and R20.9979, as shown in fig. 1.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (5)

1. A reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water comprises A, B and C, wherein the weight ratio of A: b: c-2-3: 2-3: 1-2;
the component A is a solid buffer reagent with the pH value of 9.5-11;
the component B is a mixture of a buffer reagent and a masking agent reagent;
the component C is a mixture of a filler and a calcium-magnesium reagent-acid granan K;
the component A is prepared from the following raw materials in parts by weight: adding 10g-20g of glycine, 2g-4g of lithium hydroxide, 0.1g-0.5g L-cysteine and 1g-5g of EDTA.4Na into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2-0.3g per bag to obtain a component A;
the component B is prepared from the following raw materials in parts by weight: adding 10g-20g of glycine, 2g-4g of lithium hydroxide, 0.1g-0.5g L-cysteine and 1g-5g of EGTA into a glass mortar, fully grinding until all raw materials are uniformly mixed, and then subpackaging into 0.2-0.3g of each bag to obtain a component B;
the component C is prepared from the following raw materials in parts by weight: 5g to 15g of filler polyethylene glycol, 0.5g to 1.5g of calcium magnesium reagent and 0.5g to 1.5g of acid gran K, fully grinding the raw materials until all the raw materials are uniformly mixed, and then subpackaging into 0.1g to 0.2g of each bag to obtain the component C.
2. The reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water according to claim 1, wherein:
fully grinding 10g of glycine, 3g of lithium hydroxide, 0.1g L-cysteine and 1g of EDTA.4Na until all raw materials are uniformly mixed, and then subpackaging into 0.2g of each bag to obtain a component A;
fully grinding 10g of glycine, 2g of lithium hydroxide, 0.1g of L-cysteine and 1g of EGTA until all raw materials are uniformly mixed, and then subpackaging into 0.2g of each bag to obtain a component B;
5g of polyethylene glycol 6000,0.5g of acid gran K and 0.5g of calcium-magnesium reagent, fully grinding the raw materials until all the raw materials are uniformly mixed, and then subpackaging into 0.1g of each bag to obtain the component C.
3. The reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water according to claim 1, wherein:
fully grinding 15g of glycine, 3g of lithium hydroxide, 0.25g of 0.25g L-cysteine and 4.2g of EDTA.4Na until all raw materials are uniformly mixed, and then subpackaging into 0.25g of each bag to obtain a component A;
15g of glycine, 3.2g of lithium hydroxide, 0.25g L-cysteine and 2.3g of EGTA are fully ground until all raw materials are uniformly mixed, and then the mixture is subpackaged into 0.23 g of each bag to form a component B;
7.5g of polyethylene glycol 6000,1.2g of acid gran K and 1.2g of calcium-magnesium reagent are fully ground until all raw materials are uniformly mixed, and then the raw materials are subpackaged into 0.1g of each bag to form the component C.
4. The reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water according to claim 1, wherein:
fully grinding 20g of glycine, 3g of lithium hydroxide, 0.5g L-cysteine and 5g of EDTA.4Na until all raw materials are uniformly mixed, and then subpackaging into 0.3g of each bag to obtain a component A;
20g of glycine, 4g of lithium hydroxide, 0.5g of L-cysteine and 5g of EGTA are fully ground until all raw materials are uniformly mixed, and then the raw materials are subpackaged into 0.3g of each bag to form a component B;
15g of polyethylene glycol 8000,1.2g of acid Glan K and 1.2g of calcium-magnesium reagent are fully ground until all raw materials are uniformly mixed, and then the raw materials are subpackaged into 0.2g of each bag to form the component C.
5. The use method of the reagent for rapidly detecting the hardness concentration of high-concentration magnesium in water according to claim 1, comprising the following steps:
when in use, two 10ml colorimetric bottles are taken, and water samples are respectively added to the scale marks; adding the component A into a colorimetric bottle, and shaking up to dissolve the component A to obtain a blank sample;
adding the component B into another colorimetric bottle, and shaking up to dissolve the component B to obtain a sample to be detected;
and adding two parts of the component C into two colorimetric bottles respectively, shaking uniformly for dissolving, reacting for 2min at a timing, putting a blank sample into a spectrophotometric analyzer after timing is finished, performing background calibration, and putting a sample to be detected into the spectrophotometric analyzer for reading.
CN201910922741.8A 2019-09-27 2019-09-27 Reagent for rapidly detecting magnesium hardness concentration in water and use method thereof Pending CN110646415A (en)

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CN105548177A (en) * 2016-02-19 2016-05-04 常州罗盘星检测科技有限公司 Rapid concentration detecting reagent bag for anionic polymer in water system and detecting method
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Application publication date: 20200103