CN111948196A - Method for detecting platinum ion content in solution through visual colorimetry - Google Patents
Method for detecting platinum ion content in solution through visual colorimetry Download PDFInfo
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The invention discloses a method for detecting the content of platinum ions in a solution by visual colorimetry, which comprises the following steps: and absorbing the solution to be detected by using the prepared syringe, then pushing the syringe to drop the extracting agent into the sample adding area of the filter paper, determining whether the solution to be detected contains platinum ions according to whether a color development band appears on the filter paper, and calculating the content of the platinum ions according to the length of the color development band. The detection method can realize the determination of the content of the platinum ions in the solution by visual colorimetry without detection instruments such as an ultraviolet-visible spectrophotometer and the like, and can be realized only by using an injector filled with a butyl acetate extractant and a colorimetric mixed reagent and qualitative filter paper cut into a certain specification.
Description
Technical Field
The invention belongs to the technical field of platinum ion detection methods, and particularly relates to a method for detecting the content of platinum ions in a solution through visual colorimetry.
Background
At present, the exploitation and usage amount of platinum group elements is increased year by year, and the application industries of platinum, such as jewelry, catalysts, nano materials, smelting equipment of materials and the like, are gradually increased. The platinum can be accumulated in the environment (atmospheric dust, soil and water quality), on one hand, the accumulated platinum enters plants, food, biological body fluid and animal tissues and has potential harm to human bodies and the environment, and on the other hand, the platinum can be recycled as a precious metal. The detection requirements brought by the environmental pollution and recovery based on platinum tend to be diversified, such as the rapid judgment of platinum ions in small-scale and diversified samples of jewelry cleaning solution in jewelry stores, production wastewater of processing plants, river water of monitoring stations and the like.
At present, methods for detecting platinum ions mainly include spectrophotometry, atomic absorption, atomic fluorescence, atomic emission spectrometry, mass spectrometry, and the like. However, these methods require the use of large-scale detection devices such as spectrophotometers, absorption spectrometers, emission spectrometers, mass spectrometers, etc., and some of these devices have certain requirements for samples. The detection process of the instruments is long in time consumption and high in maintenance cost, technical requirements are met for operators, and the requirements of small enterprises and individual operators on the measurement of the content of platinum ions in products or waste liquid cannot be met, and the requirements of field samples on rapid test cannot be met.
Chinese patent CN2019100298884 discloses the use of 2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride in spectrophotometric measurement of platinum. In the detection method, dilute sulfuric acid, potassium iodide, complexing agent solution and extracting agent with different concentrations or volumes are added in sequence in the complexing reaction and extraction stages, the solution preparation and detection operation are time-consuming, and the reagents are diverse and are not easy to carry; the main instrument used in the detection is an ultraviolet-visible spectrophotometer, the detection process consumes a long time and has certain technical requirements on operators. Therefore, the detection method has the defects that the detection method cannot meet the testing requirements of field samples or persons without related technical background.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a method for detecting the content of platinum ions in a solution by visual colorimetry. The invention can realize qualitative or quantitative detection of platinum ions in a field sample by using the injector and the filter paper strip, thereby simplifying the measurement process of the platinum ions, shortening the detection period and reducing the detection cost; the used articles are easy to carry, and are very suitable for field detection.
The technical scheme of the invention is specifically introduced as follows:
the invention provides a method for detecting the content of platinum ions in a solution by visual colorimetry, which comprises the following steps:
A. creation of standard color level cards
(1) Taking 10 syringes containing 5mL of butyl acetate extractant and 4mL of colorimetric mixed reagent, respectively inhaling 1mL of 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6 and 1.8 mg.L-1Pt (iv) standard solution of (2);
(2) cutting the common qualitative filter paper into 10 filter paper strips with the specification of 7mm multiplied by 85mm and one chamfered end, respectively pushing 10 syringes in the step (1) to drip 10-15 drops of butyl acetate on the sample loading area at the chamfered end of the filter paper strips, drawing lines at the cut-off position of the color development band, and obtaining the indication lines of the concentration of each platinum ion;
(3) mixing 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8 mg.L-1The indication lines of the platinum ion content are collected to form a standard color level card;
B. determination of samples
(1) Taking an injector filled with 5mL of butyl acetate extractant and 4mL of colorimetric mixed reagent, and sucking 1mL of solution to be detected;
(2) cutting common qualitative filter paper into filter paper strips with specification of 7mm multiplied by 85mm and a chamfer at one end, pushing and pressing the injector to drop 10-15 drops of butyl acetate on a sample adding area at the chamfer end of the filter paper strips, observing the existence and the length of a color developing strip, and measuring the content of platinum ions according to a standard color level card.
Further, the colorimetric mixed reagent is a mixed solution of dilute sulfuric acid, potassium iodide, sodium ascorbate and 2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride, and the mixed solution can be stored for at least 7 days under the conditions of shade and shade.
Further, the preparation of the colorimetric mixed reagent comprises: 6.25mL of 1.0mol/L dilute sulfuric acid solution, 41.50mg of KI powder, 50.00mg of sodium ascorbate powder and 7.50mL of 1.0X 10-3 mol/L2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride are transferred into a 100mL volumetric flask and the volume is determined with deionized water, wherein the reagents are not added in a fixed order.
The detection method of the invention uses the prepared injector to absorb the solution to be detected, then pushes the injector to drop the extractant into the sample adding area of the filter paper, determines whether the solution to be detected contains platinum ions according to whether the color development band appears on the filter paper, and calculates the content of the platinum ions according to the length of the color development band. The platinum-containing color development system is separated from the original liquid to be detected by using the butyl acetate extractant, so that no requirement is imposed on the color of the liquid to be detected. The used equipment is simple and easy to carry; the detection method is simple, and the technical requirements on operators are low; the method has the advantages of high measuring speed, good anti-interference performance, capability of quickly obtaining a detection result and suitability for field detection. The detection method can realize the determination of the content of the platinum ions in the solution by visual colorimetry without detection instruments such as an ultraviolet-visible spectrophotometer and the like, and can be realized only by using an injector filled with a butyl acetate extractant and a colorimetric mixed reagent and qualitative filter paper cut into a certain specification.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention uses butyl acetate extraction phase to separate the platinum-containing color development system from the original liquid to be detected, thus having no requirement on the color of the liquid to be detected.
2. The whole process of the visual colorimetric determination method can be realized by using the injector and the filter paper strip, and the visual colorimetric determination method is convenient to carry; the test method is easy to operate; the test time is short, and the detection result can be quickly obtained; large instruments and equipment are not needed, and the method is easy to popularize.
3. The standard color level card provided by the invention contains a sample adding area and nine platinum ion concentration indicating lines, can be used for quantitatively detecting each concentration of platinum ions, and has high practical application value.
4. The method for detecting the platinum ion content by visual colorimetry can be used for determining the platinum ions in mineral samples, environmental water samples, acid jewelry cleaning solution and other field samples.
Drawings
FIG. 1 is a syringe and platinum ion standard color scale card used in example 1;
fig. 2 is a result determination chart of the filter paper strip of example 3, in which: 1, background filtering paper strips; 2, adding a label filter paper strip;
fig. 3 is a result determination diagram of the filter paper strip of example 4, in which: 1, background filtering paper strips; 2, adding a label filter paper strip;
fig. 4 is a result determination chart of the filter paper strip of example 5, in which: 1, background filtering paper strips; 2, adding a label filter paper strip;
FIG. 5 is a graph showing a result judgment of the filter paper strip of example 6;
fig. 6 is a graph showing the results of determination of the filter paper strip in example 7.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1: preparation of Standard Gray cards
(1) Taking 10 syringes (shown in figure 1) containing butyl acetate extractant and colorimetric mixed reagent, and respectively inhaling 1mL of 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, and 1.8 mg.L-1Pt (iv) standard solution of (2). The original syringe was charged with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate. The colorimetric mixed reagent comprises dilute sulphuric acid, potassium iodide, sodium ascorbate and 2- [2- [4- [ (2-cyanoethyl) -methyl-amino]-phenyl radical]-vinyl radical]-1,3, 3-trimethyl-3H-indole chloride.
(2) Cutting common qualitative filter paper into 10 filter paper strips with specification of 7mm × 85mm and chamfered at one end. And pushing the injector to drop 10-15 drops of butyl acetate on the sample adding area at the chamfer end of the filter paper strip, and drawing a line at the cut-off position of the color development band to obtain the indication line of the concentration of each platinum ion.
(3) Mixing 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8 mg.L-1The platinum ion content indicator lines were summed to form a standard color scale chart. As shown in fig. 1.
Example 2: preparation of colorimetric Mixed reagents
The colorimetric mixed reagent is a mixed solution of dilute sulfuric acid, potassium iodide, sodium ascorbate and 2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride, and can be stored for at least 7 days under the conditions of shade and shade. Preparing a colorimetric mixed reagent: 6.25mL of 1.0mol/L dilute sulfuric acid solution is sucked, 41.50mg of KI powder, 50.00mg of sodium ascorbate powder and 2.58mg of 2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride are weighed out accurately and transferred to a 100mL volumetric flask, the volume is determined with deionized water and the flask is shaken well and kept in the dark. The reagents are not added in a fixed order in the preparation process.
Example 3: visual colorimetric detection of platinum ions in synthetic silicate standard substance GBW07702
A. Digestion of synthetic silicate standard: 0.1g of GBW07702 powder (synthetic silicate standard substance approved by the State technical supervision Authority, SiO) was taken2、Al2O3、CaMg(CO3)2Burning the raw materials at 950 ℃, wherein the approved value of the standard substance does not contain platinum element), adding 3mL of hydrofluoric acid and 2mL of concentrated hydrochloric acid, covering and heating at 180 ℃ until the raw materials are in a nearly dry state, and then adding 5mL of 1: 1, dispelling acid with hydrochloric acid, evaporating to dryness again, and finally diluting to 100mL with deionized water for later use.
B. Sample detection:
i. background experiment
(1) A syringe containing the butyl acetate extractant and the colorimetric mixed reagent was taken and 1mL of GBW07702 solution was aspirated. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(2) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. Pushing the syringe to drop 15 drops of butyl acetate onto the sample loading area at the chamfered end of the filter paper strip, no color band appeared, indicating no platinum ions were detected in GBW07702 solution, as shown in fig. 2-1, which also corresponds to the approved value for GBW07702 standard substance. In addition, the absence of color development band also indicates that the matrix ions in the GBW07702 standard substance do not affect the measurement result.
Labeling experiment
(1) 4.85mL of GBW07702 solution and 0.15mL 10mg·L-1Mixing Pt (IV) standard solution to obtain theoretical standard concentration of 0.3 mg.L-1The mixed solution of (1).
(2) A syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken, and 1mL of mixed solution is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(3) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. The syringe was pushed to drop 15 drops of butyl acetate onto the sample addition zone at the chamfered end of the filter paper strip, and a color band appeared, indicating that platinum ions were successfully detected in the labeled GBW07702 solution.
(4) The cut-off line of the color development band of the filter paper strip is between 0.2ppm and 0.4ppm as shown in fig. 2-2. The length of the 0.2ppm developing band is 13mm, the length of the 0.4ppm developing band is 19mm, and the length of the developing band of the marked GBW07702 solution is about 16mm, which is exactly at the midpoint between 0.2ppm and 0.4ppm, so that the platinum ion content of the marked GBW07702 solution is judged to be 0.3ppm, namely 0.3 mg.L-1. This result is consistent with the theoretical normalized concentration value. The measurement result of the labeling experiment also shows that when the synthetic silicate mineral has no platinum ions, the method can judge that the mineral has no platinum ions; when the silicate mineral contains platinum ions, even if the content is low (0.3 mg. L)-1) In the method, the content of the platinum ions can be accurately measured under the condition of coexistence of high-content matrix ions.
Example 4: visual colorimetric detection of platinum ions in argillaceous limestone standard substance GBW07108
A. Digestion of standard ore samples: taking 0.1g of GBW07108 powder (a argillaceous limestone standard substance approved by the State quality supervision, inspection and quarantine administration, wherein the natural rock mineral is obtained from argillaceous limestone in Anhui cuprum, and the approved value of the mineral does not contain platinum element), adding 3mL of hydrofluoric acid and 2mL of concentrated hydrochloric acid, covering and heating at 180 ℃ until the mixture is in a nearly dry state, and then adding 5mL of 1: 1, hydrochloric acid is used for dispelling acid, the solution is evaporated to dryness again, and finally deionized water is used for fixing the volume to 100mL for later use.
B. Sample detection:
i. background experiment
(1) A syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken and 1mL of GBW07108 solution is inhaled. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(2) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. The syringe was pushed to drop 15 drops of butyl acetate onto the sample loading area at the chamfered end of the filter paper strip, and no color band appeared, indicating that no platinum ion was detected in the GBW07108 solution, as shown in fig. 3-1. This result also corresponds to the approved value for the GBW07108 standard substance. Furthermore, the absence of a colored band also indicates the matrix ion (Si) in the GBW07108 standard4+、Al3+、Mg2+、K+、Ca2+、Ti4+、Mn4+Etc.) do not affect the measurement result.
Labeling experiment
(1) 4.30mL of GBW07108 solution and 0.70mL of 10 mg. L-1Mixing the Pt (IV) standard solution to obtain the material with the theoretical standard concentration of 1.4 mg.L-1The mixed solution of (1).
(2) A syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken, and 1mL of mixed solution is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(3) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. The syringe was pushed to drop 15 drops of butyl acetate onto the sample addition zone at the chamfered end of the filter paper strip, and a colored band appeared, indicating that platinum ions were successfully detected in the labeled GBW07108 solution.
(4) The cut-off line of the filter paper strip of the GBW07108 solution after labeling is substantially consistent with the cut-off line of 1.4ppm, and the lengths of the developed bands are all about 42mm, as shown in FIG. 3-2. Therefore, the platinum ion content in the GBW07108 solution after labeling was judged to be 1.4ppm, i.e., 1.4 mg. L-1. This result is consistent with the theoretical normalized concentration value. The measurement result of the standard addition experiment also shows that when no platinum ions exist in the natural mineral, the method can judge that no platinum ions exist in the mineral; the natural mineral contains high concentration of platinum ion (1.4 mg. L)-1) In time, the method can accurately measure the content of the platinum ions under the condition of complicated and various coexisting ions.
Example 5: visual colorimetric detection of platinum ions in river water
i. Background experiment
(1) A syringe filled with the butyl acetate extractant and the colorimetric mixed reagent is taken and 1mL of river water is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(2) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. The syringe was pushed to drop 15 drops of butyl acetate onto the sample loading area at the chamfered end of the filter paper strip, and no color band appeared, indicating that no platinum ion was detected in the river water, as shown in FIG. 4-1.
Labeling experiment
(1) 4.50mL of river water and 0.50mL of 10 mg. L-1Mixing Pt (IV) standard solution to obtain theoretical standard concentration of 1.0 mg.L-1The mixed solution of (1).
(2) A syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken, and 1mL of mixed solution is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(3) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. The syringe was pushed to drop 15 drops of butyl acetate onto the sample addition zone at the chamfered end of the filter paper strip, and a color band appeared, indicating that platinum ions were successfully detected in the added target river water.
(4) The cut-off line of the filter paper strip of the river water sample after the labeling is basically consistent with the cut-off line of 1.0ppm, and the lengths of the color development bands are all about 33mm, as shown in FIG. 4-2. Therefore, the content of platinum ions in the river water sample after the addition of the standard was judged to be 1.0ppm, that is, 1.0 mg.L-1. This result is consistent with the theoretical normalized concentration value.
Example 6: visual colorimetric detection of platinum ions in acid jewelry cleaning solution I
A. Preparing an acid jewelry cleaning solution I: 0.25mL of 100 mg. multidot.L-10.25mL of 100 mg. L of Au standard solution-10.9mL of 10 mg. multidot.L Ag standard solution-1Pt (IV) Standard solution and 3.6mL of 1.0 mol. L-1To obtain theoretical concentrations of Au, Ag and Pt of 5.0 mg.L respectively-1、5.0mg·L-1And 1.8 mg. L-1The jewelry cleaning solution I.
B. Sample detection:
(1) a syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken, and 1mL of cleaning solution I is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(2) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. And pushing the injector to drop 15 drops of butyl acetate on the sample adding area at the chamfer end of the filter paper strip, so that a color development band appears, and the platinum ions are successfully detected in the jewelry cleaning solution I.
(3) The cut-off line of the developed band of the filter paper strip was substantially identical to the cut-off line of 1.8ppm, and the length of the developed band was about 55mm, as shown in FIG. 5. Therefore, the content of platinum ions in the jewelry cleaning solution I is judged to be 1.8ppm, namely 1.8 mg.L-1. This result corresponds to the theoretical concentration value. This result also shows that the method can determine the content of platinum ions in the presence of Au and Ag.
Example 7: visual colorimetric detection of platinum ions in acid jewelry cleaning solution II
A. Preparing an acid jewelry cleaning solution II: 0.25mL of 100 mg. multidot.L-10.25mL of 100 mg. L of Au standard solution-10.1mL of 10 mg. multidot.L Ag standard solution-1Pt (IV) Standard solution and 4.4mL of 1.0 mol. L-1To obtain theoretical concentrations of Au, Ag and Pt of 5.0 mg.L respectively-1、5.0mg·L-1And 0.2 mg. L-1And jewelry cleaning solution II.
B. Sample detection:
(1) a syringe filled with the butyl acetate extractant and the colorimetric mixed reagent is taken, and 1mL of cleaning solution II is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
(2) Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. And pushing the injector to drop 15 drops of butyl acetate on the sample adding area at the chamfer end of the filter paper strip, so that a color development band appears, and the platinum ions are successfully detected in the jewelry cleaning solution II.
(3) The cut-off line of the color band of the filter paper strip substantially coincides with the cut-off line of 0.2ppm, and the lengths of the color bands are all around 13mm, as shown in FIG. 6. Therefore, the platinum ions in the jewelry cleaning solution II are judgedThe content was 0.2ppm, i.e., 0.2 mg. L-1. This result corresponds to the theoretical concentration value. This result also shows that the method has a low platinum ion content (0.2 mg. multidot.L) in the presence of Au and Ag-1) Can still be accurately measured.
Comparative example 1: spectrophotometric detection of platinum ions in N31 type neodymium phosphate glass melted by platinum crucible, inductively coupled plasma mass spectrometry detection and visual colorimetric detection of the invention
A. Sample digestion: weighing 0.2g of N31 type phosphate neodymium glass powder sample melted by a platinum crucible in a microwave digestion tank, adding 4mL of concentrated phosphoric acid and 8mL of concentrated nitric acid, and digesting for 40min at 180 ℃ in a microwave digestion instrument; after digestion, heating and evaporating on an electric heating plate until white smoke is emitted, cooling, and adding deionized water to a constant volume of 40mL to obtain digestion liquid.
B. Sample detection
(1) Spectrophotometric detection
a. Taking 1mL of digestion solution into a centrifuge tube, and sequentially adding 0.5mL of 0.5 mol.L-1H of (A) to (B)2SO4Solution, 1.0mL, 0.01 mol. L-1KI solution (containing 0.2 wt% sodium ascorbate) and 0.3mL 1X 10-3mol·L-1The complexing agent solution is added with deionized water to make the volume constant to 5mL, shaken up and kept stand for 1 min.
b. To the resulting solution was added 5mL of ethyl acetate, and after 1min of extraction, the organic phase was separated.
c. The absorbance value of the sample is measured by taking a reagent blank as a reference, and the content of the platinum is calculated and analyzed by using a standard curve y disclosed in Chinese patent 2019100298884, namely 0.3343 x-0.0056. The absorbance of the organic phase at 530nm was measured to be 0.235 by a Perkinelmer Lambda950UV-VIS-NIR UV-visible spectrophotometer, i.e., y was 0.235, and the concentration of platinum ions was calculated to be 0.72 mg.L-1。
(2) Inductively coupled plasma mass spectrometry detection
Filtering the digestion solution through a 0.22 mu m tetrafluoroethylene filter membrane, and then determining the content of platinum ions by an iCAP TQ triple quadrupole inductively coupled plasma mass spectrometer produced by Seimer Feishell science and technology company. The test adopts a KED collision reaction tank mode and selects the sameThe site element is195And (3) Pt. The content of platinum ions was 0.73 mg.L-1。
(3) Visual colorimetric detection
a. A syringe filled with a butyl acetate extractant and a colorimetric mixed reagent is taken, and 1mL of glass digestion solution is sucked. The syringe was filled with 4mL of the colorimetric mixing reagent and 5mL of butyl acetate.
b. Cutting common qualitative filter paper into filter paper strips with specification of 7mm × 85mm and chamfer at one end. And pushing the syringe to drop 15 drops of butyl acetate on the sample adding area at the chamfer end of the filter paper strip, and showing that a color development band appears, which indicates that platinum ions are successfully detected in the glass digestion solution.
c. The length of the color developing band of the filter paper strip of the glass digestion liquid is about 27 mm. The length of the developing band at 0.6ppm was 25mm, the length of the developing band at 0.8ppm was 30mm, and the length of the developing band of the filter paper strip of the glass digestion apparatus was about the midpoint between 0.6ppm and 0.8ppm, so that it was judged that the platinum ion content in the glass digestion solution was 0.7 mg.L-1。
The results of spectrophotometric detection, inductively coupled plasma mass spectrometry detection and visual colorimetric detection of platinum ions in the N31 type neodymium phosphate glass melted by the platinum crucible are respectively 0.72 mg.L-1、0.73mg·L-1And 0.7 mg. L-1. The determination results of three different methods of the same sample are basically consistent, which shows that the result obtained by the visual colorimetric detection method of the invention is reliable, and the visual colorimetric detection method has the advantages of convenience, rapidness, low cost and the like.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit of the invention, and the scope of the appended claims is to be accorded the full scope of the invention.
Claims (3)
1. A method for visually colorimetrically detecting the amount of platinum ions in a solution, comprising:
A. creation of standard color level cards
(1) Taking 10 samples, adding 5ml of butyl acetate extractant and 4ml of color comparatorThe mixed reagents were injected into a syringe containing 1mL of 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, and 1.8 mg. multidot.L-1Pt (iv) standard solution of (2);
(2) cutting the common qualitative filter paper into 10 filter paper strips with the specification of 7mm multiplied by 85mm and one chamfered end, respectively pushing 10 syringes in the step (1) to drip 10-15 drops of butyl acetate on the sample loading area at the chamfered end of the filter paper strips, drawing lines at the cut-off position of the color development band, and obtaining the indication lines of the concentration of each platinum ion;
(3) mixing 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8 mg.L-1The indication lines of the platinum ion content are collected to form a standard color level card;
B. determination of samples
(1) Taking an injector filled with 5mL of butyl acetate extractant and 4mL of colorimetric mixed reagent, and sucking 1mL of solution to be detected;
(2) cutting common qualitative filter paper into filter paper strips with specification of 7mm multiplied by 85mm and a chamfer at one end, pushing and pressing the injector to drop 10-15 drops of butyl acetate on a sample adding area at the chamfer end of the filter paper strips, observing the existence and the length of a color developing strip, and measuring the content of platinum ions according to a standard color level card.
2. The method of claim 1 for visual colorimetric detection of platinum ion content in a solution, wherein: the colorimetric mixed reagent is a mixed solution of dilute sulfuric acid, potassium iodide, sodium ascorbate and 2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride.
3. A method for visual colorimetric detection of platinum ion content in a solution in accordance with claim 2, wherein: the preparation of the colorimetric mixed reagent comprises the following steps: 6.25mL of 1.0mol/L dilute sulfuric acid solution, 41.50mg of KI powder, 50.00mg of sodium ascorbate powder and 7.50mL of 1.0X 10-3 mol/L2- [2- [4- [ (2-cyanoethyl) -methyl-amino ] -phenyl ] -vinyl ] -1,3, 3-trimethyl-3H-indole chloride are transferred into a 100mL volumetric flask and the volume is determined by deionized water.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003004533A (en) * | 2001-06-25 | 2003-01-08 | Nireco Corp | Colorimetric method and device for printed material |
| CN102109469A (en) * | 2011-03-15 | 2011-06-29 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Kit and method for detecting melamine by virtue of fast visual colorimetry |
| CN103293114A (en) * | 2012-02-22 | 2013-09-11 | 中国人民解放军海军工程大学 | Visual colorimetry for determination of phosphates |
| CN106526072A (en) * | 2016-11-24 | 2017-03-22 | 宁德师范学院 | Cd<2+> one-step detection preformed reagent and method |
| WO2019051205A1 (en) * | 2017-09-07 | 2019-03-14 | Portland State University | Hydrogel sensors for detection of metal ions |
| CN109580598A (en) * | 2017-09-28 | 2019-04-05 | 浙江化工院科技有限公司 | A kind of optical colorimetry measures the analysis method of micro acid value in fluorinated ketones contained |
| CN109632783A (en) * | 2019-01-10 | 2019-04-16 | 中国科学院上海光学精密机械研究所 | The new opplication of indoles chloride |
| CN110672597A (en) * | 2019-10-24 | 2020-01-10 | 广东省食品检验所(广东省酒类检测中心) | Propyl gallate detection test paper and detection method thereof |
-
2020
- 2020-07-16 CN CN202010685601.6A patent/CN111948196A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003004533A (en) * | 2001-06-25 | 2003-01-08 | Nireco Corp | Colorimetric method and device for printed material |
| CN102109469A (en) * | 2011-03-15 | 2011-06-29 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | Kit and method for detecting melamine by virtue of fast visual colorimetry |
| CN103293114A (en) * | 2012-02-22 | 2013-09-11 | 中国人民解放军海军工程大学 | Visual colorimetry for determination of phosphates |
| CN106526072A (en) * | 2016-11-24 | 2017-03-22 | 宁德师范学院 | Cd<2+> one-step detection preformed reagent and method |
| WO2019051205A1 (en) * | 2017-09-07 | 2019-03-14 | Portland State University | Hydrogel sensors for detection of metal ions |
| CN109580598A (en) * | 2017-09-28 | 2019-04-05 | 浙江化工院科技有限公司 | A kind of optical colorimetry measures the analysis method of micro acid value in fluorinated ketones contained |
| CN109632783A (en) * | 2019-01-10 | 2019-04-16 | 中国科学院上海光学精密机械研究所 | The new opplication of indoles chloride |
| CN110672597A (en) * | 2019-10-24 | 2020-01-10 | 广东省食品检验所(广东省酒类检测中心) | Propyl gallate detection test paper and detection method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蒙咏梅 等: ""色阶法测定食品中氰化物的含量"", 《赣南医学院学报》 * |
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