KR20230049266A - a silica detecting kit and the silica detecting method using thereof - Google Patents

Abstract

The present invention relates to a silicon concentration detection kit and a silicon concentration detection method using the same. The silicon concentration detection kit comprises a silicon bonding solution (A) comprising sodium sulfate, molybdic acid, sulfuric acid, sodium metabisulfite, and demineralized water. According to the present invention, the concentration of silicon present in trace amounts in water can be measured very accurately.

Description

Silicon concentration detection kit and silicon concentration detection method using the same {a silica detecting kit and the silica detecting method using its}

The present invention relates to a silicon (Si, silica) concentration detection method and detection kit, and more specifically, to a sample containing silicon (Si, silica) to be measured by using a silicon combine solution (Silica combine Solution) Si, silica) relates to a kit for accurately calculating the concentration and a method for calculating the silica concentration using the same.

Silica, also known as silicon dioxide (SiO2) or the mineral quartz, is a derivative compound of the chemical element silicon, making up 59% of the earth's crust, making up the largest proportion of ordinary soil. Silicon combines with oxygen to form silicates, which are the most common minerals.

Silicon (Silica) is mostly found as dissolved silica or suspended silicate particulates in natural waters. Silica is used as an additive and for water filtration in many industries, including food and pharmaceutical production processes.

Most water contains a lot of silicon and its derivative silica or silicates, and although concentrations above 100 mg/L are not uncommon, silica concentrations in water are generally less than 30 mg/L and exceed 1000 mg/L. Concentration can be found in salt water and saline water.

Silica can cause significant problems in industrial water, and silica and silicates are added to water as conditioners, detergents, and corrosion inhibitors. However, silica in water can cause serious problems in industrial fields, especially boilers and steam fields, and silica accumulates in boiler tubes and heat exchangers at high pressure and high temperature.

These glassy deposits reduce the efficiency of heat exchangers and lead to premature failure, and silica builds up on steam turbine blades, reducing efficiency and costly downtime for cleaning. Silica levels should therefore be kept below 0.005 mg/L (5 ppb) in ultra-high pressure applications.

Measuring silica in the water is used to monitor the efficiency of the desalter, while testing for silica (one of the first impurities detected when the desalter's exchange capacity is exhausted) can check the sensitivity of the desalter's performance. there is.

In this way, due to the importance of silicon, it is very important to accurately measure silicon, and the method of measuring silicon is measured by the following method.

absorbance photometry

go. principle

Silicic acid reacts with ammonium molybdate at an acidity around Ph1.2 to form a silicon molybdate complex. It is reduced with aminonaphtholsulfanic acid to form blue heteropoly blue, which is colorimetrically measured.

me. Experiment method

A) Sample storage and pretreatment

It is recommended to measure the number of samples immediately after collection, but when sample storage is necessary, it is better to put it in a polyethylene bottle and store it in a cool and dark place, and this should not exceed 5 days.

b) preparation

- Spectrophotometer

-Hydrochloric acid (1+1) solution

-Ammonium molybdate solution

: ((NH ₄ )6Mo7O ₂ 4).4H ₂ Dissolve 10 g of O in 100 ml of distilled water. If this solution is not adjusted to pH 7-8 using silicon silicate-free ammonia water or sodium hydroxide solution, precipitation occurs. In addition, if the solution is stored in a glass bottle, the silicic acid will dissolve, so it is stored in a polyethylene bottle.

- oxalic acid solution

: Dissolve 7.5 g of H ₂ C ₂ O ₄ .9H ₂ O in 100 ml of distilled water.

- Reduction reagent

: Dissolve 1-amino-2-naphthol-4-sulfanic acid and 1g sodium hypochlorite (Na ₂ SO ₃ ) in 50ml of distilled water. Combine this solution with 150 ml of 20% NaSO4 solution. Store in a cool dark place and throw away when it turns black.

-Standard stock solution of silicon silicate

: Weigh 4.73g of sodium metasilicate (Na ₂ SiO ₃ .9H ₂ O) and dissolve it in a distillation pot to make 1 liter and store it in a polyethylene bottle.

- Silicon silicate standard solution

: Take 25ml of the standard stock solution, add distilled water, dilute to 250ml, and pour into a polyethylene bottle. The concentration of this solution is 1000 mg/l SiO ₂ -Si

c) analysis process

: For 50ml sample water, add 1ml hydrochloric acid and 2ml ammonium molybdate solution, mix well and leave for 5-10 minutes. Add 2 ml oxalic acid solution to this, add 2 ml reducing reagent after 2-15 minutes, mix well, and after 5 minutes, measure the absorbance at 815 nm wavelength with distilled water as a control, and obtain the silicon silicate activity from a calibration curve prepared separately. The absorbance measurement is corrected by the absorbance of the blank test solution using distilled water.

D) Preparation of calibration curve

Take 0.2-5.0ml of silicon silicate standard solution step by step and add distilled water to dilute to 100ml to make a solution with a concentration of 2-50mg/l SiO ₂ -Si. After measuring the absorbance by treating these solutions in the same way as the sample number, prepare a calibration curve after correcting the absorbance of the blank test solution.

As a prior art related to measuring silicon, Korean Patent Publication No. 10-2011-0040851 (silicon concentration measuring device) discloses "an excitation light irradiation unit 2 for irradiating excitation light for silicon to a test liquid; and A silicon concentration measurement comprising a light detection unit 3 for detecting fluorescence and/or scattered light emitted from silicon in the test liquid and a calculation unit 41 for calculating the silicon concentration in the test liquid from the intensity of the fluorescence and/or scattered light. device" was presented.

The prior art and prior art described above have disadvantages in that the measuring process is very complicated due to various reagents and complicated procedures for measuring the silicon concentration of a sample, and that it is not economical in terms of cost and takes a long measurement time due to the use of various reagents. there is,

The present invention was derived by solving the problems of the prior art and the prior art, and the measurement process is very complicated with various reagents and complicated procedures in measuring the silicon concentration of the sample, which is a problem of the prior art, and also uses various reagents. It is intended to provide a silicon concentration detection kit and a silicon concentration detection method using the same, which are not economical in terms of cost but also improve the disadvantages of taking a long measurement time.

In addition, the present invention is sometimes affected by interference by other types of ions included in the sample when measuring the silicon concentration using a detection reagent for detecting the silicon concentration in the prior art, which is significantly improved. It is intended to provide a concentration detection kit and a silicon concentration detection method using the same.

In order to solve the above problems and needs, the present invention

Contains a silicon bond solution (A) composed of sodium sulfate, molybdic acid, sulfuric acid, sodium metabisulfite, and demineralized water Provided is a silicon concentration detection kit configured by.

In addition, the present invention, the silicon bonding solution (A) is sodium sulfate (Sodium sulfate) 100 parts by weight of molybdic acid (Molybdic acid) 30 to 70 parts by weight, sulfuric acid (Sulfuric acid) 30 to 70 parts by weight, It provides a silicon concentration detection kit, characterized in that it is composed by mixing 150 to 350 parts by weight of sodium metabisulfite and 500 to 1000 parts by weight of distilled water.

In addition, the present invention is a step of mixing the silicon-binding solution (A) of the silicon concentration detection kit with a sample containing silicon to be measured to develop color (step 1),

The process of creating a calibration curve for the standard solution (step 2),

Provided is a silicon concentration measuring method including a process (three steps) of measuring the concentration of silicon contained in the sample by putting the color-developed measurement sample into a measuring container by mixing the above sample and the silicon-binding solution (A).

The silicon concentration detection kit and the silicon concentration detection method using the same according to the present invention have the effect of very accurately measuring the silicon concentration present in water in a small amount.

The silicon concentration detection kit and the silicon concentration detection method using the same according to the present invention have the effect of significantly excluding the influence of interference by other types of ions that may occur during silicon measurement.

In addition, the silicon-binding solution (A) used in the silicon concentration detection kit and the silicon concentration detection method using the same according to the present invention dramatically shortens the reaction time with silicon, so that excessive measurement time is not required and the procedure can be performed very simply. effect appears.

1 is an embodiment of a calibration curve for a standard solution according to the present invention.
Figure 2 is a flow chart of a silicon concentration detection method using a silicon concentration detection kit according to the present invention.

Hereinafter, the present invention will be described in detail with reference to the drawings.

The present invention relates to a silicon concentration detection kit used when using a spectrophotometric method or a colorimetric contrast method, which is a representative method for measuring the concentration of silicon (Si, silica) contained in a sample.

In the present invention, the detection kit is a device or device for measuring or analyzing water quality, and means a device or equipment for analyzing water quality using a detection reagent, and more specifically, a sample such as the absorbance photometry method and the colorimetric comparison method described above. It means a device or equipment that can analyze water quality through physical and chemical changes such as color change of water.

In addition, the present invention relates to a method for detecting the concentration of silicon using a spectrophotometric method or a colorimetric contrast method, which is a representative method for measuring the concentration of silicon contained in a sample using a silicon concentration detection kit.

The present invention provides a silicon concentration detection kit comprising a silicon binding solution (A).

The silicon-binding solution (A) of the present invention means a chemical or reagent that functions to form a silicon compound by interacting with silicon included in a sample and to cause the formed silicon compound to develop color.

The silicon-bonding solution (A) of the present invention contains sodium sulfate, molybdic acid, sulfuric acid, sodium metabisulfite, and demineralized water. means a solution prepared by

Preferably, the silicon bonding solution (A) of the present invention contains 30 to 70 parts by weight of molybdic acid, 30 to 70 parts by weight of sulfuric acid, 100 parts by weight of sodium sulfate, It is effective to mix 150 to 350 parts by weight of sodium metabisulfite and 500 to 1000 parts by weight of distilled water.

Sodium sulfate of the present invention is sodium sulfate, which is a sulfate of sodium, and is a white crystal made by heating sodium chloride with concentrated sulfuric acid or neutralizing sodium carbonate and sulfuric acid. It is used to make glass or ultramarine blue. . Its chemical formula is Na2SO4.

Molybdic acid of the present invention has the formula MoO3·H2O or MoO3·2H2O. As MoO3·H2O, it is slightly soluble in water (2.05 g/ℓ, 23℃) and can be obtained in the form of a sol. MoO3·2H2O is a monoclinic columnar crystal and is soluble in water, but difficult to obtain from aqueous solutions. It becomes MoO3·H2O in concentrated sulfuric acid dryer or at 50~65℃.

These compounds are hydrates of molybdenum oxide, MoO3 2H2O shares the vertices of the MoO6 octahedron and contains connected layers, one H2O coordinates to Mo and the other H2O to hydrogen in a lattice. are combined It can be obtained from a strong nitric acid solution of molybdate or a hydrochloric acid solution of MoO3. At room temperature, yellow MoO3·2H2O crystallizes very slowly. And in the hot solution, MoO3·H2O, which is a pale yellow crystal, is rapidly formed.

Sulfuric acid of the present invention is an anti-acid, and sulfuric acid is a strongly acidic liquid compound. Except for water, it is the most manufactured and used in many places. Sulfuric acid with high concentrations (more than about 90% by mass) is called concentrated sulfuric acid or concentrated sulfuric acid. Concentrated sulfuric acid has weak properties as an acid. Instead, it acts as a strong acid dehydration because of its strong hygroscopicity. If it comes into contact with organic matter, it absorbs hydrogen and oxygen in the form of water molecules. Sulfuric acid burns if it comes into contact with the skin. Burns are caused by this dehydration and heat.

Sodium metabisulfite of the present invention is a substance widely used as a preservative and antioxidant as chemical formula Na2S2O5, sodium metabisulfite, sodium metabisulfite (Sodium Metabisulfite, Sodium Metabisulphite).

Sodium metabisulfite is the common name for sodium bisulfite, and an aqueous solution can be obtained by passing sulfur dioxide through a saturated solution of sodium carbonate. It has strong reducing power, and is usually used as an aqueous solution at a concentration of 100 g/ℓ and is used as a reducing agent in chromium wastewater treatment.

As described above, the silicon measurement method according to the conventional water quality conservation method is measured by the absorbance photometry method.

The present invention is a method of measuring the concentration of silicon by mixing the silicon-binding solution (A) according to the above-described silicon concentration detection kit with a sample containing silicon to be measured to develop color, and then using an absorbance photometry method and a colorimetric comparison method. to provide.

In the present invention, a process of developing color by mixing a sample containing silicon to be measured and a silicon binding solution (A) is performed. (Step 1)

Mixing 0.5 to 5 parts by weight of the silicon-binding solution (A) with 100 parts by weight of the silicon-containing sample shows the effect of improving the color development of the sample.

The reaction time of mixing the silicon-containing sample and the silicon-binding solution (A) is preferably about 1 to 8 minutes, preferably about 5 minutes.

In the present invention, a process of preparing a calibration curve for a standard solution is performed. (Step 2)

The calibration curve is prepared by adding and mixing the silicon-bonded solution (A) of the present invention by mixing it with samples whose silicon concentrations are presented in each step.

The present invention mixes the above sample and the silicon-bonded solution (A) in a measuring container, puts the colored measurement sample into the measuring container, measures the absorbance at the measured wavelength, and compares it with the calibration curve for the above standard solution to determine the level of silicon contained in the sample. The process of measuring the concentration is performed. (Step 3)

As already mentioned, the spectrophotometric method used in the present invention refers to a conventional method of obtaining the concentration of the target component by changing the target component in the sample solution into a light absorbing material with an appropriate reagent and measuring the degree of light absorption at a specific wavelength. .

The measurement wavelength of the spectrophotometry of the present invention is preferably 880 nm.

The absorbance spectrophotometric method of the present invention calculates the concentration of the target component by applying Lambert Beer's law, and a conventional absorbance spectrophotometer usually consists of a light source unit, a wavelength selection unit, a sample unit, and a light metering unit.

Methods for measuring the concentration in the absorbance photometry include a colorimetric method using the degree of color development and a nephelometry method using the degree of suspension of the sample solution. In the absorbance photometry method, a control solution corresponding to a sample solution is prepared, the absorbance is measured, a calibration curve is prepared accordingly, and the absorbance of the sample solution is measured and the concentration is measured by comparing the absorbance with the calibration curve.

In the present invention, both the colorimetric table and the turbidity method can be used, and preferably, the colorimetric table method has high accuracy.

In addition, the colorimetric table comparison method is as follows.

As described above, standard solutions are prepared according to various concentrations of the desired component, and a standard colorimetric table is set by adding the silicon-bonded solution (A) of the present invention to the standard solutions.

And it means a method of measuring the concentration of the sample solution by comparing the degree of color development obtained by mixing and mixing the silicon-bonded solution (A) with the sample with the standard colorimetric table.

Therefore, in the present invention, any method of mixing and reacting the silicon-binding solution (A) of the present invention with a sample and measuring the concentration using the degree of color development will be included in the technical content of the present invention.

<Example>

1. Manufacturing method of silicon bonding solution (A)

Reagent 1.

Synonyms: sodium sulfate

CAS No.: 7681-38-1

reagent 2.

Synonyms: Molybdic acid

CAS No.: 7782-91-4

reagent 3.

Synonyms: Sulfuric acid

CAS No.: 7664-93-9

reagent 4.

Synonyms: sodium metabisulfite

CAS No.: 7681-57-4

reagent 5.

Synonyms: Demineralized water

CAS No.: 7732-18-5

The composition ratio of each reagent in the silicon-binding solution (A) is shown in [Table 1] below.

Reagent # reagent 1 reagent 2 reagent 3 reagent 4 reagent 5 Weight ratio (%) 10 5 5 20 70

2. Silicon concentration detection method

(1) Use of spectrophotometric method

1) 1 ml (about 1 mg) of the silicon-binding solution (A) prepared above is mixed with 10 ml of a silicon-containing sample and reacted to induce color development.

The reaction time was about 5 minutes.

The above sample is measured using an absorbance photometry method.

Measurement wavelength: 880 nm, and the measurement vessel is a round glass bottle with a diameter of 1 Inch.

2) Prepare a calibration curve for the standard solution.

The calibration curve is prepared by adding and mixing the silicon-bonded solution (A) of the present invention by mixing it with samples whose silicon concentrations are presented in each step.

The calibration curve of the control solution for the standard solution is as shown in FIG.

An accurate silicon concentration is measured by comparing the absorbance of the sample with the calibration curve of the control solution.

(2) Colorimetric comparison method

As described above, a colorimetric table for the standard solution is prepared and the concentration of silicon is calculated by comparing the degree of color development of the sample in which the color development is induced.

As shown in Table 2 below, the present invention shows a high limit that can exclude the influence of ion interference.

Therefore, it can be seen that the use of the silicon detection method according to the present invention has the effect of significantly reducing the effect of interference by other types of ions included in the sample.

interfering substances Threshold (mg/l) Calcium 100 mg/l Chloride 100 mg/l Ferric ion All levels Nitrite All levels Strong oxidizing/reducing substances All levels

The present invention provides a silicon concentration detection kit for measuring the concentration of silicon present in water having the above configuration and functions, and a silicon concentration detection method using the same.

The present invention can be widely used in water purification and wastewater treatment business, pollution prevention business, education business, etc. related to the Framework Act on Water Quality Environment.

In addition, the present invention can be widely used in the pollution prevention monitoring industry, national and local government environmental policy related industries, and the like.

In addition, it is a very useful invention for water quality analysis drug business, water quality analysis drug manufacturing business, environmental supervision business, environmental modeling business, environmental impact assessment business, and educational material provision business.

In particular, the present invention is very useful for industries producing, manufacturing, processing, distributing, and researching devices for measuring silicon concentration.

Claims (3)

Contains a silicon bond solution (A) composed of sodium sulfate, molybdic acid, sulfuric acid, sodium metabisulfite, and demineralized water A silicon concentration detection kit constructed by
According to claim 1,
The silicon bonding solution (A) is 30 to 70 parts by weight of molybdic acid, 30 to 70 parts by weight of sulfuric acid, and sodium metabisulfite in 100 parts by weight of sodium sulfate. (Sodium metabisulfite) 150 to 350 parts by weight, distilled water (Demineralized water) 500 to 1000 parts by weight of a mixture characterized in that the composition is a silicon concentration detection kit.
Process of mixing the silicon-binding solution (A) of the silicon concentration detection kit according to claim 1 or 2 with a sample containing silicon to be measured to develop color (Step 1);
The process of creating a calibration curve for the standard solution (step 2),
A method for measuring silicon concentration comprising mixing the above sample and the silicon binding solution (A) and measuring the concentration of silicon contained in the sample by putting the colored measurement sample into a measuring container (step 3).

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