CN111458330A - Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof - Google Patents
Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof Download PDFInfo
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- CN111458330A CN111458330A CN202010349828.3A CN202010349828A CN111458330A CN 111458330 A CN111458330 A CN 111458330A CN 202010349828 A CN202010349828 A CN 202010349828A CN 111458330 A CN111458330 A CN 111458330A
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- 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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- 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
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Abstract
The embodiment of the invention discloses a method for semi-quantitatively detecting content of metasilicic acid in mineral water and a detection reagent thereof, wherein the reagent comprises ammonium molybdate tetrahydrate and ammonium bisulfate, the concentration of the ammonium molybdate tetrahydrate is 4.0-4.2 g/L, and the concentration of the ammonium bisulfate is 9.0-9.4 g/L on the basis of a water sample to be detected.
Description
Technical Field
The embodiment of the invention relates to the technical field of detection of metasilicic acid content, in particular to a method for semi-quantitatively detecting the content of metasilicic acid in mineral water and a detection reagent thereof.
Background
GB 8537 Natural mineral Water for drinking uses metasilicic acid as one of the limit indexes, and requires that the content of metasilicic acid cannot be lower than 25 mg/L if metasilicic acid is taken as the evaluation standard.
Currently, the detection of metasilicic acid in water is mainly carried out according to "silicomolybdenum yellow spectrometry" and "silicomolybdenum blue spectrometry" in GB 8538 "inspection method for Natural mineral Water for Drinking", wherein the concentration ranges of calibration curve points of the two methods are "0-20 mg/L" and "0-2 mg/L", respectively, and the concentration points of the calibration curve do not cover the minimum concentration required when metasilicic acid is used as a limit index in GB 8537.
Disclosure of Invention
Therefore, the embodiment of the invention provides a method for semi-quantitatively detecting the content of metasilicic acid in mineral water and a detection reagent thereof, which realize the semi-quantitative analysis of the content directly in a colorimetric mode by adopting reasonable reagent compatibility, avoid the operation by adopting a spectrophotometer, enable the experimental operation to be more convenient and quicker, can detect at any time and any place, simultaneously avoid the use of reagents such as hydrochloric acid and the like, and avoid potential safety threat.
In order to achieve the above object, an embodiment of the present invention provides the following:
the invention provides a metasilicic acid detection reagent, which comprises ammonium molybdate tetrahydrate and ammonium bisulfate, wherein the concentration of the ammonium molybdate tetrahydrate is 4.0-4.2 g/L, and the concentration of the ammonium bisulfate is 9.0-9.4 g/L based on a water sample to be detected.
As a preferable scheme of the invention, the reagent further comprises oxalic acid, and the concentration of the oxalic acid is 2.5-3.0 g/L based on the water sample to be detected.
The invention also provides a method for semi-quantitatively detecting the content of metasilicic acid in mineral water, which adopts the detection reagent and comprises the following steps:
s100, preparing metasilicic acid standard solutions with different concentrations respectively, adding the reagent into each standard solution respectively, mixing, and oscillating until color development is achieved to obtain the RGB value of the standard solution under each concentration; comparing the standard chromaticity cards under the state of locking the G value, controlling the deviation of the R values of a plurality of standard solutions to be not higher than 7, adjusting the B value to obtain the RGB standard value of each standard solution, and preparing the metasilicic acid standard colorimetric card;
s200, adding the reagent into a water sample to be tested, mixing, and oscillating to develop color to obtain a test solution to be compared;
s300, comparing the test solution to be compared with a metasilicic acid standard colorimetric card, and correspondingly obtaining the content of metasilicic acid according to the color.
As a preferable embodiment of the present invention, in step S100, the concentration of the standard solution of metasilicic acid is, in order by gradient, 5 mg/L, 15 mg/L, 25 mg/L, 35 mg/L, 45 mg/L, 55 mg/L, and 65 mg/L.
In a preferred embodiment of the present invention, the color development in step S100 and step S200 is yellow.
As a preferred scheme of the present invention, the method is to use a colorimetric box for operation, the colorimetric box comprises a comparison portion and a reagent storage portion, the comparison portion comprises a colorimetric card holding cavity and a colorimetric cavity which are sequentially arranged along a vertical direction, and the colorimetric card holding cavity and the colorimetric cavity are separated by a transparent sheet;
the reagent storage part is provided with a plurality of reagent storage cavities which are sequentially arranged along the length direction of the comparison part, and each reagent storage cavity can be communicated with the colorimetric cavity.
In a preferred embodiment of the present invention, a sealing plate capable of opening or closing the reagent storage chamber is provided on an upper surface of each of the reagent storage chambers, a through hole is provided on a side surface of each of the reagent storage chambers adjacent to the colorimetric chamber, and a sealing cover is detachably provided on the through hole.
As a preferable scheme of the present invention, the colorimetric cavity is further provided with a water outlet.
As a preferable scheme of the invention, the content of metasilicic acid in the detected mineral water is 5-65 mg/L.
The embodiment of the invention has the following advantages:
1) the content of metasilicic acid in water is semi-quantitatively analyzed by adopting a color comparison mode of a color comparison card, so that the experiment operation is more convenient and quicker, the operation is not required to be carried out by using a spectrophotometry, and the effect of quickly detecting the content of metasilicic acid at any time and any place is realized;
2) various raw materials in the reagent used in the test are powder, so that the reagent is convenient to carry and operate on the spot in a water source; meanwhile, hydrochloric acid and the like are not needed, so that potential safety threats to experimenters in the process of preparing and using reagents are avoided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a flow chart of a method for semi-quantitatively detecting the content of metasilicic acid in mineral water according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a colorimetric box according to an embodiment of the present invention;
fig. 3 is a top view of a colorimetric cartridge according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a reagent storage chamber according to an embodiment of the present invention
Fig. 5 is a metasilicic acid standard color chart according to an embodiment of the present invention.
In the figure:
1-contrasting portion; 2-a reagent storage section;
11-a colorimetric card placing cavity; 12-a colorimetric cavity; 13-a transparent sheet;
21-a reagent storage chamber;
121-water outlet;
211-a sealing plate; 212-through hole.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 4, the invention provides a metasilicic acid detection reagent, which comprises ammonium molybdate tetrahydrate and ammonium bisulfate, wherein the concentration of the ammonium molybdate tetrahydrate is 4.0 to 4.2 g/L, and the concentration of the ammonium bisulfate is 9.0 to 9.4 g/L based on the water sample to be detected.
In a further preferred embodiment, in order to further avoid the interference of phosphate in a water sample to be detected, the reagent further comprises oxalic acid, and the concentration of the oxalic acid is 2.5-3.0 g/L by taking the water sample to be detected as a reference.
Of course, specifically, in a more preferred embodiment, the concentration of ammonium molybdate tetrahydrate is further limited to 4.000 g/L, the concentration of ammonium bisulfate is further limited to 9.209 g/L, and the concentration of oxalic acid is 2.800 g/L based on the sample water to be tested, further, each of the above-mentioned specific detection raw materials can be prepared into reagent packs respectively for convenient carrying, and since the volume of the collected sample water to be tested is controllable, the specific content of each reagent pack can be converted according to the volume thereof, for example, in practice, the volume of the sample water to be tested is generally selected to be 20m L, based on which 0.080g of ammonium molybdate tetrahydrate, 0.184g of ammonium bisulfate and 0.056g of oxalic acid can be weighed and prepared into reagent packs respectively, and A, B and C are respectively identified for distinction, and the number of each reagent pack can be reasonably prepared according to circumstances.
As shown in fig. 1-4, the present invention also provides a method for semi-quantitatively detecting the content of metasilicic acid in mineral water, using the reagent according to the above, the method comprising:
s100, preparing metasilicic acid standard solutions with different concentrations respectively, adding the reagent into each standard solution respectively, mixing, and oscillating until color development is achieved to obtain the RGB value of the standard solution under each concentration; comparing the standard chromaticity cards under the state of locking the G value, controlling the deviation of the R values of a plurality of standard solutions to be not higher than 7, adjusting the B value to obtain the RGB standard value of each standard solution, and preparing the metasilicic acid standard colorimetric card;
s200, adding the reagent into a water sample to be tested, mixing, and oscillating to develop color to obtain a test solution to be compared;
s300, comparing the test solution to be compared with a metasilicic acid standard colorimetric card, and correspondingly obtaining the content of metasilicic acid according to the color.
In a further preferred embodiment, in step S100, the concentration of the standard solution of metasilicic acid is, in order by gradient, 5 mg/L, 15 mg/L, 25 mg/L, 35 mg/L, 45 mg/L, 55 mg/L and 65 mg/L.
In a more preferred embodiment, the color development in step S100 and step S200 is yellow.
Of course, in order to make the whole operation more convenient and faster, in a preferred embodiment, the method is to use a colorimetric box for operation, the colorimetric box comprises a comparison portion 1 and a reagent storage portion 2, the comparison portion 1 comprises a colorimetric card placing cavity 11 and a colorimetric cavity 12 which are sequentially arranged along a vertical direction, and the colorimetric card placing cavity 11 and the colorimetric cavity 12 are separated by a transparent sheet 13; the reagent storage portion 2 is formed with a plurality of reagent storage chambers 21 arranged in sequence along the longitudinal direction of the counterpart 1, and each of the reagent storage chambers 21 is capable of communicating with the colorimetric chamber 12. Further, a sealing plate 211 capable of opening or closing the reagent storage chamber 21 is provided on an upper surface of each of the reagent storage chambers 21, a through hole 212 is provided on a side surface of each of the reagent storage chambers 21 adjacent to the colorimetric chamber 12, and a sealing cover is detachably provided on the through hole 212. Simultaneously, in order to make the water sample that awaits measuring after the detection can conveniently pour out, still be provided with apopore 121 on the color comparison chamber 12, of course, can set up the detachable closing cap on the apopore 121 here to make and avoid its outflow scheduling problem in mixing the in-process.
Through the setting, make can place the water sample that awaits measuring in color comparison chamber 12 to open one of them reagent according to the circumstances and deposit chamber 21, let reagent and the water sample that awaits measuring mix and shake through shaking evenly to the water sample colouration that awaits measuring, because the color comparison card is placed and is separated through transparency 13 between chamber 11 and the color comparison chamber 12, consequently, the color that is located color comparison card and is placed color comparison chamber 12 of chamber 11 below can directly compare with metasilicic acid standard color comparison card, improves the accuracy of reading. Of course, the color chart placing cavity 11 can also be directly drawn by pigment, so as to avoid the white part caused by directly placing the common color chart.
In a further preferred embodiment, the content of metasilicic acid in the detected mineral water is 5-65 mg/L.
The preparation process of the metasilicic acid standard colorimetric card is specifically described below. Wherein, ammonium molybdate tetrahydrate, ammonium bisulfate and metasilicic acid are analytically pure, and water is tertiary water specified in GB/T6682.
A standard solution of metasilicic acid was prepared at a concentration of 100. mu.g/m L.
Respectively sucking metasilicic acid standard solutions 2m L, 6m L, 10m L0, 14m L1, 18m L2, 22m L3 and 26m L4, respectively placing the metasilicic acid standard solutions in polyethylene vials, and respectively diluting the metasilicic acid standard solutions to 40m L by using water to obtain metasilicic acid solutions with the concentrations of 5 mg/L, 15 mg/L, 25 mg/L, 35 mg/L, 45 mg/L, 55 mg/L and 65 mg/L;
0.160g of ammonium molybdate tetrahydrate and 0.368g of ammonium bisulfate are respectively added into each part of the obtained metasilicic acid solution, and the mixture is fully oscillated until the color is developed;
the L, a, and b values of the developed metasilicic acid solution were measured using a spectrocolorimeter at 10 degrees in a projection mode (wherein each concentration was measured three times), and the results are shown in table 1;
converting the L ab value into an RGB value, locking the G value, comparing the color difference between the paper colorimetric card (i.e. the standard colorimetric card) and the developed metasilicic acid solution under the condition of sufficient light, finely adjusting the R value, and adjusting the B value in a gradient manner to finally obtain the RGB reference value of the metasilicic acid standard colorimetric card, wherein the result is shown in Table 2, and the prepared metasilicic acid standard colorimetric card is shown in FIG. 5.
TABLE 1
TABLE 2
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The metasilicic acid detection reagent is characterized by comprising ammonium molybdate tetrahydrate and ammonium bisulfate, wherein the concentration of the ammonium molybdate tetrahydrate is 4.0-4.2 g/L and the concentration of the ammonium bisulfate is 9.0-9.4 g/L based on the water sample to be detected.
2. The metasilicic acid detection reagent of claim 1, wherein the reagent further comprises oxalic acid, and the concentration of the oxalic acid is 2.5-3.0 g/L based on the water sample to be detected.
3. A method for semi-quantitatively detecting the content of metasilicic acid in mineral water, using the reagent according to claim 1 or 2, the method comprising:
s100, preparing metasilicic acid standard solutions with different concentrations respectively, adding the reagent into each standard solution respectively, mixing, and oscillating until color development is achieved to obtain the RGB value of the standard solution under each concentration; comparing the standard chromaticity cards under the state of locking the G value, controlling the deviation of the R values of a plurality of standard solutions to be not higher than 7, adjusting the B value to obtain the RGB standard value of each standard solution, and preparing the metasilicic acid standard colorimetric card;
s200, adding the reagent into a water sample to be tested, mixing, and oscillating to develop color to obtain a test solution to be compared;
s300, comparing the test solution to be compared with a metasilicic acid standard colorimetric card, and correspondingly obtaining the content of metasilicic acid according to the color.
4. The method of claim 3, wherein the concentration of the metasilicic acid standard solution is 5 mg/L, 15 mg/L, 25 mg/L, 35 mg/L, 45 mg/L, 55 mg/L and 65 mg/L in sequence according to a gradient in the step S100.
5. The method of claim 3 or 4, wherein the colors of the mineral water are yellow in steps S100 and S200.
6. The method for semi-quantitatively detecting the content of metasilicic acid in mineral water according to claim 3 or 4, wherein the method is performed by using a colorimetric box, the colorimetric box comprises a comparison portion (1) and a reagent storage portion (2), the comparison portion (1) comprises a colorimetric card placing cavity (11) and a colorimetric cavity (12) which are sequentially arranged along a vertical direction, and the colorimetric card placing cavity (11) and the colorimetric cavity (12) are separated by a transparent sheet (13);
the reagent storage part (2) is provided with a plurality of reagent storage cavities (21) which are sequentially arranged along the length direction of the comparison part (1), and each reagent storage cavity (21) can be communicated with the colorimetric cavity (12).
7. The method of claim 6, wherein a sealing plate (211) for opening or closing the reagent storage chamber (21) is disposed on an upper surface of each reagent storage chamber (21), and a through hole (212) is disposed on a side surface of each reagent storage chamber (21) adjacent to the colorimetric chamber (12), and a sealing cover is detachably disposed on the through hole (212).
8. The method for semi-quantitatively detecting the content of metasilicic acid in mineral water according to claim 7, wherein the colorimetric cavity (12) is further provided with a water outlet hole (121).
9. The method of claim 3 or 4, wherein the content of metasilicic acid in the mineral water is 5-65 mg/L.
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Cited By (1)
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