CN109212074B - Method for detecting strontium content in methyl tin mercaptide - Google Patents
Method for detecting strontium content in methyl tin mercaptide Download PDFInfo
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Abstract
The invention discloses a method for detecting strontium content in methyl tin mercaptide. The method comprises the following steps: (1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using mixed acid liquor to obtain digestion liquor; (2) neutralizing the digestion solution by using alkali liquor to obtain a neutralization solution, and mixing the neutralization solution with an extracting agent to obtain an extracting solution; (3) performing constant volume and filtration treatment on the extracting solution to obtain a solution to be detected; (4) and detecting the liquid to be detected by using an ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result. The method for detecting the strontium content in the methyl tin mercaptide has the advantages of simple sample pretreatment and high detection result accuracy.
Description
Technical Field
The invention relates to the field of analytical chemistry, in particular to a method for detecting strontium content in methyl tin mercaptide.
Background
The methyl tin mercaptide is an important chemical raw material and is widely applied to the fields of PVC films, sheets, building materials, medical appliances and the like, the content of metal elements in PVC products is extremely strict, and the influence of the content of other metal elements on PVC materials is also extremely large except common heavy metal elements.
The methyl tin mercaptide is not flammable and belongs to an organic product, and for the detection of the content of metal elements in the methyl tin mercaptide, if Atomic Absorption Spectroscopy (AAS) or Atomic Emission Spectroscopy (AES) such as atomic emission spectroscopy (ICP-AES) taking high-frequency inductively coupled plasma as a light source is used, the pretreatment of a sample is quite complicated; if the flame stability is directly influenced by the sample itself in the machine test.
Thus, the existing means for detecting metal elements in methyl tin mercaptide still need to be improved.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. To this end, an object of the present invention is to propose a method for detecting the strontium content in methyltin mercaptides. The method for detecting the strontium content in the methyl tin mercaptide has the advantages of simple sample pretreatment and high detection result accuracy.
In one aspect of the invention, the invention provides a method for detecting the strontium content in methyl tin mercaptide. According to an embodiment of the invention, the method comprises: (1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using mixed acid liquor to obtain digestion liquor; (2) neutralizing the digestion solution by using alkali liquor to obtain a neutralization solution, and mixing the neutralization solution with an extracting agent to obtain an extracting solution; (3) performing constant volume and filtration treatment on the extracting solution to obtain a solution to be detected; (4) and detecting the liquid to be detected by using an ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result.
According to the method for detecting the strontium content in the methyltin mercaptide, firstly, a mixed acid solution is utilized to digest a methyltin mercaptide sample to be detected, so that strontium ions are dissolved out; neutralizing the digestion solution by using alkali liquor, and extracting the dissolved strontium ions by using an extracting agent to obtain an extracting solution; the extracting solution is subjected to simple constant volume and filtration treatment to obtain a solution to be detected; and then carrying out ion chromatography detection on the solution to be detected, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result. The method is simple to operate, consumes less time, generates less pollution in the detection process, has high accuracy and is suitable for detecting the strontium content in the methyl tin sample.
In addition, the method for detecting the strontium content in methyl tin mercaptide according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the present invention, the mixed acid solution comprises sulfuric acid and nitric acid. Therefore, the dissolution rate of strontium ions in the sample to be detected can be obviously improved, and the accuracy of the detection result is improved.
In some embodiments of the invention, the volume ratio of the sulfuric acid to the nitric acid in the mixed acid solution is 1 (1-10). Therefore, the dissolution rate of strontium ions in the sample to be detected can be further improved, and the accuracy of the detection result is further improved.
In some embodiments of the invention, the lye is an aqueous sodium hydroxide solution.
In some embodiments of the invention, the pH value of the neutralization solution is 6-8. Therefore, the strontium can be further extracted by the extractant, and the accuracy of the detection result is further improved.
In some embodiments of the invention, the extractant is an aqueous acetonitrile solution. Thereby, the extraction of strontium from the sample can be further facilitated.
In some embodiments of the invention, the concentration of the acetonitrile aqueous solution is 5-15 v%. Thereby, the extraction of strontium from the sample can be further facilitated.
In some embodiments of the invention, the detection conditions of the ion chromatography comprise: the particle size of the cation exchange column packing is 3 mu m; the temperature of the column oven is 40 ℃; the temperature of the conductivity detector is 40 ℃; the suppression current is 20 mA; the leacheate comprises 1.0-4.4 mmol/L methanesulfonic acid; the sample injection amount is 20-30 mu L; the flow rate is 0.5-1.0 mL/min. This can further improve the accuracy of the detection result.
In some embodiments of the invention, the leacheate further comprises 0.5-2.0 mmol/L18-crown-6. This can further improve the accuracy of the detection result.
In some embodiments of the invention, the leacheate comprises 3.0mmol/L methanesulfonic acid and 1.0 mmol/L18-crown-6. This can further improve the accuracy of the detection result.
In some embodiments of the invention, the method of detecting methyl tin mercaptide comprises: (1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using a mixed acid solution of sulfuric acid and nitric acid to obtain a digestion solution; the volume ratio of the sulfuric acid to the nitric acid is 1:5, and the ratio of the mixed acid liquid to the methyl tin mercaptide sample to be detected is 4mL:1 g; (2) neutralizing the digestion solution by using a 10 wt% sodium hydroxide aqueous solution until the pH value is 6-8 to obtain a neutralized solution, and mixing the neutralized solution with a 10 v% acetonitrile aqueous solution for ultrasonic extraction to obtain an extracting solution; (3) after the extracting solution is subjected to constant volume by using ultrapure water, sequentially passing the obtained sample through a solid-phase extraction small column and a needle type filtering membrane to obtain a solution to be detected; (4) detecting the liquid to be detected by ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result; wherein the detection conditions of the ion chromatography comprise: the particle size of the cation exchange column packing is 3 mu m; the temperature of the column oven is 40 ℃; the temperature of the conductivity detector is 40 ℃; the suppression current is 20 mA; the leacheate comprises 3.0mmol/L methanesulfonic acid and 1.0 mmol/L18-crown-6; the sample injection amount is 25 mu L; the flow rate was 0.7 mL/min. Therefore, the method is simple to operate, consumes less time, generates less pollution in the detection process, has high accuracy and is suitable for detecting the strontium content in the methyl tin sample.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
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The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a chromatogram of a mixture of sodium, potassium, magnesium, calcium and strontium ions in example 1;
FIG. 2 is a chromatogram obtained by mixing and amplifying sodium ions, potassium ions, magnesium ions, calcium ions and strontium ions in example 1;
FIG. 3 is a chromatogram of a methyl tin mercaptide sample to be tested in example 1;
FIG. 4 is a linear plot of strontium ion concentration versus chromatographic peak area for example 1.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In one aspect of the invention, the invention provides a method for detecting the strontium content in methyl tin mercaptide. According to an embodiment of the invention, the method comprises: (1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using mixed acid liquor to obtain digestion liquor; (2) neutralizing the digestion solution by using alkali liquor to obtain a neutralization solution, and mixing the neutralization solution with an extracting agent to obtain an extracting solution; (3) performing constant volume and filtration treatment on the extracting solution to obtain a solution to be detected; (4) and (3) detecting the liquid to be detected by ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result.
According to the method for detecting the strontium content in the methyltin mercaptide, firstly, a mixed acid solution is utilized to digest a methyltin mercaptide sample to be detected, so that strontium ions are dissolved out; neutralizing the digestion solution by using alkali liquor, and extracting the dissolved strontium ions by using an extracting agent to obtain an extracting solution; the extracting solution is subjected to simple constant volume and filtration treatment to obtain a solution to be detected; and then carrying out ion chromatography detection on the solution to be detected, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result. The method is simple to operate, consumes less time, generates less pollution in the detection process, has high accuracy and is suitable for detecting the strontium content in the methyl tin sample.
According to the embodiment of the invention, in the step (1), the type of the mixed acid solution used for performing the digestion treatment on the methyl tin mercaptide sample to be measured is not particularly limited, and can be selected by a person skilled in the art according to actual needs. According to the embodiment of the invention, the methyl tin mercaptide sample to be measured can be digested by using the mixed acid solution containing sulfuric acid and nitric acid, so that the dissolution of strontium ions and the elimination of other interfering substances in the sample can be further facilitated. In addition, the inventor finds in experiments that a mixed acid solution of sulfuric acid and nitric acid is more suitable for digesting the methyl tin mercaptide sample than other common digestion acids (such as a mixed acid system of hydrochloric acid, hydrofluoric acid, perchloric acid and the like), which is probably because the methyl tin mercaptide is a viscous organic substance and contains longer carbon chains, the intramolecular carbon chains of the methyl tin mercaptide are difficult to open by common non-oxidizing acids, and the carbon chains of the organic substance can be opened by the combined use of concentrated sulfuric acid and nitric acid which have strong oxidizing property and acidity. In addition, sulfuric acid and nitric acid are relatively safe compared to perchloric acid, which is easily explosive when heated.
According to an embodiment of the invention, the volume ratio of the sulfuric acid to the nitric acid in the mixed acid solution is 1 (1-10), for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9 or 1: 10. Wherein, the sulfuric acid and the nitric acid can be directly products of superior grade pure concentrated sulfuric acid and concentrated nitric acid which are obtained from the market. Therefore, the dissolution rate of strontium ions in the sample to be detected can be further improved, and the accuracy of the detection result is further improved. The inventor finds that the digestion effect of the methyl tin mercaptide sample to be detected is obviously influenced by the volume ratio of sulfuric acid to nitric acid in the mixed acid solution, the effective dissolution of strontium ions in the methyl tin mercaptide can not be ensured due to the excessively low volume ratio of the nitric acid, in addition, the volume of the nitric acid is excessively low, and is relatively high, and in the pretreatment and acid dispelling processes, a large amount of white smoke is emitted by the sulfuric acid, so that a small amount of ions to be detected can be taken away, and the accuracy of a detection result is further influenced; secondly, the generated dense smoke has strong irritation and corrosiveness, and can cause certain damage and pollution to human bodies and the environment. If the volume of the nitric acid is too high, dehydration performance of the mixed acid solution is possibly reduced due to too low volume ratio of the sulfuric acid, interfering substances in a sample to be detected cannot be effectively eliminated, and accuracy of a detection result is affected. Furthermore, the inventor finds that the dissolution of strontium ions in a methyl tin mercaptide sample to be detected is facilitated and the interference impurities in the sample can be effectively eliminated by controlling the volume ratio of sulfuric acid to nitric acid in the mixed acid solution to be within the range of 1 (1-10), so that the detection result is ensured to have higher accuracy.
According to the embodiment of the present invention, in the step (2), the kind of the alkali solution used for neutralizing the digestion solution is not particularly limited, and those skilled in the art can select the alkali solution according to actual needs. According to a specific embodiment of the present invention, the digestion solution may be neutralized with an aqueous sodium hydroxide solution. Therefore, the acidic digestion solution can be effectively neutralized, and other ions which possibly interfere the detection can not be introduced into the digestion solution, so that the detection result is further ensured to have higher accuracy. According to the embodiment of the present invention, the concentration of the sodium hydroxide aqueous solution is not particularly limited, and for example, the sodium hydroxide concentration may be 5 to 20 wt%. If the concentration of the sodium hydroxide is too low, a large amount of sodium hydroxide aqueous solution is needed to complete the neutralization of the digestion solution, so that the detection efficiency is influenced, and the constant volume is influenced; if the concentration of sodium hydroxide is too high, the aqueous sodium hydroxide solution becomes too viscous, the workability is poor, and it is difficult to control the point of neutralization by adjusting the degree of neutralization of the digestion solution by the amount of the aqueous sodium hydroxide solution added. The inventor finds that the use amount of the alkali liquor can be controlled in a proper range by adopting a 5-20 wt% sodium hydroxide aqueous solution to neutralize the digestion liquor, and the method is more suitable for regulating and controlling the pH value of the terminal point of neutralization of the digestion liquor. According to a specific example of the present invention, the concentration of the aqueous sodium hydroxide solution is 10 wt%, thereby facilitating the neutralization of the digestion solution.
According to the specific example of the invention, after the methyl tin mercaptide sample to be detected is digested, the digestion solution can be heated to remove acid, and then subsequent neutralization is carried out. Specifically, the digestion solution may be heated to drive acid by methods well known to those skilled in the art, for example, the digestion solution may be heated at 110 ℃ for 30min to discharge the excessive acid solution in the digestion solution, thereby not only effectively reducing the usage of the alkali solution in the neutralization treatment, but also greatly reducing the adverse effect of the excessive acid solution on the subsequent detection result.
According to the embodiment of the invention, the pH value of the digestion solution can be adjusted to 2-10 by using the alkali liquor. The above pH range provides a beneficial acidity adjustment for the extraction of strontium ions by the extractant, avoiding the loss of strontium ions due to the extraction process. According to the preferred embodiment of the invention, the pH value of the digestion solution can be adjusted by using the alkali liquor until the pH value of the obtained neutralization solution is 6-8. Therefore, the pH value of the neutralization solution is controlled within the range of 6-8, so that the strontium can be further extracted by the subsequent extractant, and the accuracy of the detection result is further improved.
According to an embodiment of the present invention, in the step (3), strontium in the neutralized solution may be extracted using an extraction agent (e.g., an organic solvent) commonly used in the art. According to a specific embodiment of the present invention, acetonitrile may be used as the extractant. Preferably, the extractant may be acetonitrile in water. Acetonitrile has excellent solvent performance, can dissolve various organic and inorganic substances, can be infinitely mutually soluble with water and alcohol, and the low-concentration acetonitrile aqueous solution can not cause damage to a chromatographic column.
Thus, extraction of strontium from a sample may be further facilitated according to embodiments of the present invention, and the concentration of the acetonitrile aqueous solution may be 5-15 v%. The inventor finds that the impurity peak in the sample peak is reduced in the subsequent detection process along with the increase of the acetonitrile concentration, but the performance of the chromatographic column is influenced by the excessively high acetonitrile concentration. More preferably, the concentration of the aqueous acetonitrile solution is 10 v%. Therefore, the extraction of strontium in the sample can be further facilitated, and the accuracy of the detection result can be further improved.
According to a specific example of the present invention, in the process of extracting strontium by using the extracting agent, the sample may be subjected to ultrasonic oscillation for 10-45 min, preferably 20 min. If the time of ultrasonic oscillation is too short, strontium ions cannot enter the extractant sufficiently, and the accuracy of the detection result is affected. If the ultrasonic oscillation time is too long, the experimental efficiency is reduced. This further improves the extraction rate of strontium from the sample. And after the extraction is finished, fixing the volume of the sample by using water, passing the sample after the volume fixing through a solid phase extraction small column, removing macromolecular organic matters in the sample, and passing through a needle type filter membrane to obtain the liquid to be detected.
According to the embodiment of the invention, in the step (4), the solution to be detected is subjected to ion chromatography detection, and based on the detection result, the strontium content in the methyl tin mercaptide sample to be detected can be determined through a standard curve method. The detection conditions of the ion chromatography include: the particle size of the cation exchange column packing is 3 mu m; the temperature of the column oven is 40 ℃; the temperature of the conductivity detector is 40 ℃; the suppression current is 20 mA; the leacheate comprises 1.0-4.4 mmol/L methanesulfonic acid; the sample injection amount is 20-30 mu L; the flow rate is 0.5-1.0 mL/min. The inventor proves in experiments that the particle size of the exchange column is too large, the column effect of the chromatographic column is too low, the peak is widened and shortened, the particle size is too small, and the column pressure is too high; in addition, the retention time of ions to be detected is too long due to too low concentration of the leacheate, the separation degree of the ions to be detected is reduced due to too high concentration of the leacheate, and the chromatographic column packing is damaged; moreover, too high flow rate can cause the column pressure of the chromatographic column to rise, the separation degree of ions to be detected becomes poor, and too low flow rate can cause the peak time of the ions to be detected to be too long. Furthermore, the inventor optimizes the chromatographic conditions through a large amount of experiments, and the accuracy of the detection result can be further improved and the service life of the chromatographic column can be prolonged by detecting the sample under the chromatographic conditions.
According to the embodiment of the invention, the leacheate can further comprise 0.5-2.0 mmol/L18-crown-6. This can further improve the accuracy of the detection result. Crown ethers are macrocyclic ligands having a hydrophilic internal cavity and a hydrophobic external portion, within which a metal ion can form a stable complex with the cavity. The radius of an inner hole of the 18-crown ether-6 is 1.38nm, and the radius of potassium ions is also 1.38nm, so that the potassium ion retention effect is strong. The peak time of K ions can be changed by adjusting the concentration of the strontium ions, so that the potassium ions and the strontium ions can be well separated.
According to an embodiment of the present invention, the leacheate may comprise 3.0mmol/L methanesulfonic acid and 1.0 mmol/L18-crown-6. This can further improve the accuracy of the detection result.
In conclusion, the method for detecting the strontium content in the methyl tin mercaptide provided by the embodiment of the invention is simple to operate, consumes less time, generates less pollution in the detection process, has high accuracy, and is suitable for detecting the strontium content in the methyl tin samples.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
(1) The apparatus used and the chromatographic conditions:
the instrument comprises the following steps: IC6200 ion chromatograph, cation suppressor, and conductivity detector manufactured by Anhui Instrument science and technology Limited; AS3100 auto sampler.
Chromatographic conditions are as follows:
a chromatographic column: cation exchange chromatography column, 4.6 x 150 mm;
leacheate: 3.0mmol/L methanesulfonic acid solution +1.0 mmol/L18-crown-6;
flow rate: 0.7 mL/min;
column temperature: 40 ℃;
the temperature of the pool is as follows: 40 ℃;
suppression of current: 20 mA;
sample introduction amount: 25 μ L.
(2) Pretreatment of methyltin sample
Accurately weighing 3.0012g of methyl tin mercaptide sample, placing the sample in a high-pressure digestion tank liner, adding 2mL of sulfuric acid and 10mL of nitric acid, reacting for 2h at 130 ℃, taking out a polytetrafluoroethylene liner, placing the polytetrafluoroethylene liner on an electric heating plate to remove acid until about 5mL of sample solution remains, cooling, adding 10 wt% of sodium hydroxide solution to adjust the pH value to 6.9, adding 10mL of 10 v% of acetonitrile aqueous solution, performing ultrasonic oscillation for 20min in an ultrasonic cleaning machine, extracting oily substances in the sample, cooling, adding ultrapure water, and fixing the volume to 100 mL.
And (3) taking an RP pretreatment column, activating by using high-grade pure methanol, then slowly passing a sample through the RP column to remove a large amount of macromolecular organic matters, and passing through a 0.45-micrometer needle type filter membrane to obtain the liquid to be tested for the computer test.
(3) Preparation of leacheate
198 mu L of superior pure methanesulfonic acid is accurately measured, 0.2670g of the superior pure 18-crown-6 reagent is measured, dissolved and transferred to a 1000mL volumetric flask, the volume is fixed to a scale by ultrapure water, and the volumetric flask is placed in an ultrasonic cleaning machine for ultrasonic degassing for 20min after suction filtration.
(4) Preparation of Standard solutions
Accurately weighing 0.02mL, 0.05mL, 0.1mL, 0.15mL and 0.2mL of Sr standard solution with the concentration of 1000 mug/mL, respectively, placing the Sr standard solution into a 100mL volumetric flask for mixing, and fixing the volume to scale by using ultrapure water to obtain the Sr ion standard solution with the concentration of 0.2 mug/mL, 0.5 mug/mL, 1.0 mug/mL, 1.5 mug/mL and 2.0 mug/mL.
Simultaneously preparing a mixed standard solution containing sodium ions, potassium ions, magnesium ions, calcium ions and strontium ions, wherein the sodium ion concentration is 2.0. mu.g/mL, 4.0. mu.g/mL, 8.0. mu.g/mL, 10.0. mu.g/mL, 20.0. mu.g/mL, the potassium ion concentration is 0.5. mu.g/mL, 1.0. mu.g/mL, 2.0. mu.g/mL, 3.0. mu.g/mL, 4.0. mu.g/mL, the magnesium ion concentration is 2.0. mu.g/mL, 4.0. mu.g/mL, 8.0. mu.g/mL, 10.0. mu.g/mL, 20.0. mu.g/mL, the calcium ion concentration is 5.0. mu.g/mL, 10.0. mu.g/mL, 15.0. mu.g/mL, 20.0. mu.g/mL, 40.0. mu.g/mL, the strontium ion concentration is 0. mu.g/mL, 0. mu.5. g/mL, 1.0. mu.g/mL, 1.0. mu.0 g/mL, 1.0 g/mL, 2.0. mu.g/mL.
(5) Analysis of Sr ion Standard solution
The prepared Sr ion standard solution with the concentration of 0.2 mug/mL, 0.5 mug/mL, 1.0 mug/mL, 1.5 mug/mL and 2.0 mug/mL enters an ion chromatographic system for analysis according to the principle that the concentration is from low to high, so as to obtain a linear equation (the linear relation is shown in figure 4) of the concentration and the peak area, and the linear correlation coefficient is 0.999. Meanwhile, the mixed standard solution containing sodium ions, potassium ions, magnesium ions, calcium ions and strontium ions is analyzed, and the chromatograms are shown in fig. 1 and fig. 2.
(6) Detection of Sr ions in methyltin mercaptide sample
Respectively placing the blank sample, the sample and the standard sample into an automatic sample injector sample cup, detecting according to the chromatographic conditions in the step (1) to obtain a detection spectrogram of strontium ions in the methyltin mercaptide sample, as shown in fig. 3, calculating the content of Sr ions in the sample according to a linear equation of the Sr ions, and performing a standard recovery rate experiment according to the content of Sr, wherein the experimental results are shown in table 1:
TABLE 1 sample recovery test results
The result shows that the method for detecting the strontium content in the methyl tin mercaptide has good accuracy.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (6)
1. A method for detecting the strontium content in methyl tin mercaptide is characterized by comprising the following steps:
(1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using mixed acid liquor to obtain digestion liquor;
(2) neutralizing the digestion solution by using alkali liquor to obtain a neutralized solution, mixing the neutralized solution with an extracting agent, and extracting the dissolved strontium ions by using the extracting agent to obtain an extracting solution;
(3) performing constant volume and filtration treatment on the extracting solution to obtain a solution to be detected;
(4) detecting the liquid to be detected by ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result;
the mixed acid solution consists of sulfuric acid and nitric acid, and the volume ratio of the sulfuric acid to the nitric acid in the mixed acid solution is 1 (1-10);
the pH value of the neutralization solution is 6-8;
the detection conditions of the ion chromatography comprise:
the particle size of the cation exchange column packing is 3 mu m;
the temperature of the column oven is 40 ℃;
the temperature of the conductivity detector is 40 ℃;
the suppression current is 20 mA;
the leacheate comprises 1.0-4.4 mmol/L methanesulfonic acid;
the sample injection amount is 20-30 mu L;
the flow rate is 0.5-1.0 mL/min;
the leacheate further comprises 0.5-2.0 mmol/L18-crown ether-6.
2. The method of claim 1, wherein the alkaline solution is an aqueous solution of sodium hydroxide.
3. The method of claim 1, wherein the extractant is an aqueous acetonitrile solution.
4. The method according to claim 3, wherein the concentration of the aqueous acetonitrile solution is 5 to 15 v%.
5. The method of claim 1, wherein the leacheate comprises 3.0mmol/L methanesulfonic acid and 1.0 mmol/L18-crown-6.
6. A method for detecting the strontium content in methyl tin mercaptide is characterized by comprising the following steps:
(1) carrying out digestion treatment on a methyl tin mercaptide sample to be detected by using a mixed acid solution of sulfuric acid and nitric acid to obtain a digestion solution; the volume ratio of the sulfuric acid to the nitric acid is 1:5, and the ratio of the mixed acid liquid to the methyl tin mercaptide sample to be detected is 4mL:1 g;
(2) neutralizing the digestion solution by using a 10 wt% sodium hydroxide aqueous solution until the pH value is 6-8 to obtain a neutralized solution, and mixing the neutralized solution with a 10 v% acetonitrile aqueous solution for ultrasonic extraction to obtain an extracting solution;
(3) after the extracting solution is subjected to constant volume by using ultrapure water, sequentially passing the obtained sample through a solid-phase extraction small column and a needle type filtering membrane to obtain a solution to be detected;
(4) detecting the liquid to be detected by ion chromatography, and determining the strontium content in the methyl tin mercaptide sample to be detected based on the detection result; wherein the detection conditions of the ion chromatography comprise:
the particle size of the cation exchange column packing is 3 mu m;
the temperature of the column oven is 40 ℃;
the temperature of the conductivity detector is 40 ℃;
the suppression current is 20 mA;
the leacheate comprises 3.0mmol/L methanesulfonic acid and 1.0 mmol/L18-crown-6;
the sample injection amount is 25 mu L;
the flow rate was 0.7 mL/min.
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