CN111537657A - Method for detecting content of trace metal ions in high-purity thiourea by ion chromatography - Google Patents
Method for detecting content of trace metal ions in high-purity thiourea by ion chromatography Download PDFInfo
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- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 title claims abstract description 74
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004255 ion exchange chromatography Methods 0.000 title claims abstract description 29
- 229910021655 trace metal ion Inorganic materials 0.000 title claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims abstract description 25
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims abstract description 7
- 239000011591 potassium Substances 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 7
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims abstract description 4
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 16
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 14
- 239000012488 sample solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 238000010812 external standard method Methods 0.000 claims description 6
- 238000012417 linear regression Methods 0.000 claims description 6
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 6
- 229910001414 potassium ion Inorganic materials 0.000 claims description 6
- 239000012086 standard solution Substances 0.000 claims description 5
- 238000005341 cation exchange Methods 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- 238000004445 quantitative analysis Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 15
- 150000001768 cations Chemical class 0.000 abstract description 4
- -1 calcium cations Chemical class 0.000 abstract description 3
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012224 working solution Substances 0.000 abstract description 2
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- MVXMNHYVCLMLDD-UHFFFAOYSA-N 4-methoxynaphthalene-1-carbaldehyde Chemical compound C1=CC=C2C(OC)=CC=C(C=O)C2=C1 MVXMNHYVCLMLDD-UHFFFAOYSA-N 0.000 description 2
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- LBVNUQQORDPZCR-UHFFFAOYSA-N calcium;sulfane Chemical compound S.[Ca] LBVNUQQORDPZCR-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- YAECNLICDQSIKA-UHFFFAOYSA-L calcium;sulfanide Chemical compound [SH-].[SH-].[Ca+2] YAECNLICDQSIKA-UHFFFAOYSA-L 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
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Abstract
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for detecting the content of trace metal ions in high-purity thiourea by ion chromatography. Detecting sodium, ammonium, potassium, magnesium and calcium cations by adopting an ion chromatography, preparing a standard working solution by utilizing five cation standard samples, establishing a standard curve by using the response peak area of the metal ion standard sample as a vertical coordinate and the ion content as a horizontal coordinate according to the response of metal ions in a cation system, substituting the response peak area of corresponding ions in the sample into the standard curve, and calculating the content of the metal ions in the sample. The method has the advantages of simple operation, rapid detection, no need of complex pretreatment, no toxicity and harm in the detection process, high accuracy and good reproducibility.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for detecting the content of trace metal ions in high-purity thiourea by ion chromatography.
Background
Thiourea, white and lustrous crystals. Is bitter in taste. Melting point 176-. Dissolved in water. Is easy to deliquesce in air, and can be used as dye and dyeing assistant for synthetic medicine. The detection standard currently used is HGT3266-2022, and no ion detection method is involved in this standard. Therefore, the ion content of the domestic thiourea is not detected at present.
The prior thiourea production process comprises the steps of absorbing hydrogen sulfide gas through lime cream under negative pressure to prepare a calcium hydrogen sulfide solution, reacting the calcium hydrogen sulfide solution with calcium cyanamide, wherein the molar ratio of calcium hydrosulfide to calcium cyanamide is 1:5, continuously stirring, filtering under negative pressure to obtain thiourea liquid, and concentrating and crystallizing the thiourea liquid to obtain the thiourea. The high-purity thiourea sold in the market at present is prepared by recrystallization. The impurity content is extremely low, and the thiourea contains a very small amount of soluble impurities and is difficult to detect by other methods.
Disclosure of Invention
In order to solve the technical problems, the invention adopts ion chromatography to detect sodium, ammonium, potassium, magnesium and calcium cations, five cation standard samples are utilized to prepare standard working solution, according to the response of metal ions in a cation system, the response peak area of the metal ion standard sample is used as a vertical coordinate, the ion content is used as a horizontal coordinate to establish a standard curve, the response peak area of corresponding ions in the sample is brought into the standard curve, and the metal ion content in the sample is calculated. The method has the advantages of simple operation, rapid detection, no need of complex pretreatment, no toxicity and harm in the detection process, high accuracy and good reproducibility.
The invention relates to a method for detecting the content of trace metal ions in high-purity thiourea by ion chromatography, which comprises the following steps:
1) drawing an ion chromatography standard curve: respectively preparing standard mixed solutions with the ion contents of sodium, ammonium, potassium, magnesium and calcium of 0.01ppm, 0.05ppm, 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm, injecting the mixed solutions by using an automatic sample injector, carrying out quantitative analysis by using an external standard method, carrying out linear regression analysis on the chromatographic peak area of a target compound and the corresponding concentration to obtain a standard curve linear regression equation, wherein the correlation coefficient of the curve is more than or equal to 0.995;
the specific standard mixed solution can be prepared by the following method:
taking 10ml of sodium, ammonium, potassium, magnesium and calcium ion standard solutions of 1000ppm respectively, diluting to 100ml with water, preparing 100ppm standard mixed solution, and then preparing 0.01ppm, 0.05ppm, 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm standard mixed solution respectively.
2) And (3) determining the ion content in the thiourea sample: dissolving high-purity thiourea by using first-grade water, preparing a sample solution, injecting a sample by using an automatic sampler, measuring to obtain the peak area of a target object, quantifying by using an external standard method, substituting into a linear regression equation, and calculating the content of metal ions in a sample to be measured.
The sample amount in the steps 1) and 2) is 500 mu L, and the concentration of the sample solution of the high-purity thiourea is 0.08-0.1g/ml in general; the ion chromatography is used for detecting the content of ppm, because the ion content is extremely low, the response value is increased by increasing the sample volume (adopting a quantitative ring of 500 uL), but the excessive sample volume needs a matched quantitative ring, the existing chromatographic instrument is not suitable for use, so that the accuracy and the normal detection are influenced, and the excessive thiourea concentration also increases the dissolution difficulty and influences the detection result, so that the detection standard curve is in a normal corresponding range. If the thiourea product with lower purity is obtained, the detection can be carried out by the method, so that the concentration or the sample amount of the sample solution can be properly reduced, and the thiourea content is ensured to be in the range.
Preferably, the sample solution is filtered through a 0.22 μm filter before use;
the carbon dioxide is removed before the primary water is used, the conductivity is less than or equal to 0.05mS/m, and the contents of suspended matters, particles and ions are extremely low, so that the requirements of the ion chromatographic column packing are met, meanwhile, the background conductivity value in the detection process is reduced, and the signal-to-noise ratio is improved.
In the process of drawing an ion chromatography standard curve and measuring the ion content in a sample, the column temperature is 30-35 ℃, the flow rate is 0.6-1.0mL/min, the analysis time is 25min or more, and the leacheate can be 12-16mmol/L methane sulfonic acid aqueous solution.
The suppressor current is set according to the concentration of the leacheate, and is generally set according to about three times of the numerical value of the concentration of the leacheate (wherein the concentration of the leacheate is mmol/L, and the current is mA).
More preferably, during steps 1) and 2): the column temperature is 30 ℃, the flow rate is 1.0mL/min, and the leacheate is 16mmol/L methane sulfonic acid aqueous solution.
The column temperature is an optimal value, the service life of the chromatographic column is prolonged, and the optimal temperature of the column effect is maintained; the eluent concentration influences the ion peak time, and the use of a 16mmol/L methane sulfonic acid eluent is optimal, at which each ion can be well separated.
Filtering the standard mixed solution and the sample solution in the steps 1) and 2) by using an organic RP small column before sample injection.
In the ion chromatography system employed in the present invention: the protection column is CG12A protection column with size of 4 × 50 mm; the analytical column adopts a CS12A cation exchange column with the size of 4 multiplied by 250 mm; the model of the suppressor is CERS500, and the size is 4 mm; the ion chromatography system also includes conventional configurations such as an autosampler, an ion chromatography pump, a six-way valve, a conductivity detector, a data processing system, and the like.
The method for detecting the metal ions in the thiourea sample is simple and rapid, and a large number of experiments prove that the method has high precision and accuracy of standard addition recovery, and the test result is accurate and reliable.
Drawings
FIG. 1 is a standard curve of sodium ion in examples 1 and 2;
FIG. 2 standard graph of ammonium ion in examples 1 and 2;
FIG. 3 standard curve of potassium ion in examples 1 and 2;
FIG. 4 is a graph of the standard curve of magnesium ion in examples 1 and 2;
FIG. 5 standard curve of calcium ion in examples 1 and 2;
FIG. 6 is a graph showing the appearance of peaks of five metal ions in Experimental example 1;
FIG. 7 is a graph showing the appearance of peaks of five metal ions in Experimental example 2;
in fig. 6 and 7, the peaks appearing from left to right are sodium ion, ammonium ion, potassium ion, magnesium ion, and calcium ion, respectively.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but it should not be construed that the scope of the above subject matter is limited to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention, and the following embodiments are all completed by adopting the conventional prior art except for the specific description.
Example 1
The content of five metal ions of a batch of high-purity thiourea solid samples needs to be detected.
The ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS600, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 1.0mL/min, a suppressor current of 47mA, a sample injection amount of 500 muL, an analysis time of 25min and a leacheate of 16mmol/L methane sulfonic acid aqueous solution.
The method adopts an ion chromatograph to carry out detection and quantitative analysis by an external standard method, and comprises the following specific steps:
(1) drawing an ion chromatography standard curve: preparing sodium, ammonium, potassium, magnesium and calcium ion standard solutions, wherein the concentration is 1000 mg/l; transferring 10.00mL of each metal ion standard solution into a 100mL volumetric flask by using a pipette, shaking the solution with constant volume uniformly to obtain 100ppm of standard mixed solution A, and diluting a proper amount of the standard mixed solution A by corresponding times to obtain standard mixed solutions with the concentrations of 0.01ppm, 0.05ppm, 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm respectively.
Respectively shaking up standard mixed solutions with different concentrations, injecting samples by using an ion chromatography automatic sample injector, wherein the sample injection amount is 500 mu L, and drawing an ion standard solution concentration-peak area standard curve after all standard samples are operated to obtain a corresponding standard curve regression equation (see figures 1, 2, 3, 4 and 5);
in FIG. 1, the formula:
y is peak area in mus min;
x is the concentration of sodium ions, and the unit is mg/L;
r: a linear correlation coefficient.
In FIG. 2, the formula:
y is peak area in mus min;
x is the concentration of ammonium ions, and the unit is mg/L;
r: a linear correlation coefficient.
FIG. 3 is a schematic diagram of: y is peak area in mus min;
x is the concentration of potassium ions, and the unit is mg/L;
r: a linear correlation coefficient.
In FIG. 4, the formula: y is peak area in mus min;
x is the concentration of magnesium ions, and the unit is mg/L;
r: a linear correlation coefficient.
FIG. 5 is a graph of: y is peak area in mus min;
x is the concentration of calcium ions, and the unit is mg/L;
r: a linear correlation coefficient.
(2) And (3) determining the ion content in the thiourea sample:
accurately weighing 6 parts of 0.8g thiourea sample to 0.0001g, diluting the sample to a constant volume of 10mL volumetric flask with first-grade water except carbon dioxide, and filtering by using an RP (reverse osmosis) column to prepare 6 parts of solution to be detected. The same chromatographic conditions were used for quantitative loop injection at 500 μ L on the same ion chromatograph, while the peak area was recorded.
(3) Calculation of Metal ion content
The content of each metal ion is calculated according to a standard curve regression equation (detailed in figures 1-5), and the experimental data and the detection results are detailed in table 1:
TABLE 1
Example 2
A batch of common thiourea solid samples different from the sample in the example 1 is tested for the content of five metal ions:
the ion chromatography conditions employed were: the device comprises an automatic sample injector, an ion chromatographic pump, a six-way valve, a protective column CG12A, a size of 4 x 50mm, an analytical column CS12A cation exchange column, a size of 4 x 250mm, a suppressor model of CERS500, a size of 4mm, a conductivity detector, a data processing system, a column temperature of 30 ℃, a flow rate of 1.0mL/min, a suppressor current of 47mA, a sample injection amount of 500 muL, an analysis time of 25min and a leacheate of 16mmol/L methane sulfonic acid aqueous solution.
The method adopts an ion chromatograph to carry out detection and quantitative analysis by an external standard method, and comprises the following specific steps:
(1) drawing an ion chromatography standard curve: same as example 1
(2) Preparing thiourea sample solution
Accurately weighing 6 parts of 0.80g guanidine hydrochloride sample, accurately measuring to 0.0001g, fixing the volume in a 100mL volumetric flask, and filtering by using an RP (RP) small column to prepare 6 parts of solution to be measured. The same chromatographic conditions were used for quantitative loop injection at 500 μ L on the same ion chromatograph, while the peak area was recorded.
(3) Calculation of Metal ion content
The experimental data and the detection results are detailed in table 2:
TABLE 2
Claims (9)
1. A method for detecting the content of trace metal ions in high-purity thiourea by ion chromatography is characterized by comprising the following steps:
1) drawing an ion chromatography standard curve: respectively preparing standard mixed solutions with the ion contents of sodium, ammonium, potassium, magnesium and calcium of 0.01ppm, 0.05ppm, 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm, injecting the mixed solutions by using an automatic sample injector, carrying out quantitative analysis by using an external standard method, carrying out linear regression analysis on the chromatographic peak area of a target compound and the corresponding concentration to obtain a standard curve linear regression equation, wherein the correlation coefficient of the curve is more than or equal to 0.995;
2) and (3) determining the ion content in the thiourea sample: dissolving high-purity thiourea by using first-grade water, preparing a sample solution, injecting a sample by using an automatic sampler, measuring to obtain the peak area of a target object, quantifying by using an external standard method, introducing the peak area into a unitary linear regression equation, and calculating the content of metal ions in a sample to be measured;
the sample amount in the steps 1) and 2) is 500 mu L, and the concentration of the sample solution in the step 2) is 0.08-0.1 g/ml.
2. The method for detecting the content of the trace metal ions in the high-purity thiourea by the ion chromatography as claimed in claim 1, wherein in the steps of drawing the ion chromatography standard curve in the step 1) and measuring the ion content in the thiourea sample in the step 2), the column temperature is 30-35 ℃, the flow rate is 0.6-1.0mL/min, the analysis time is 25min or more, and the leacheate can be 12-16mmol/L methane sulfonic acid aqueous solution.
3. The method for detecting the content of the trace metal ions in the high-purity thiourea by ion chromatography according to claim 2, wherein in the processes of the steps 1) and 2): the column temperature is 30 ℃, the flow rate is 1.0mL/min, and the leacheate is 16mmol/L methane sulfonic acid aqueous solution.
4. The method for detecting the content of the trace metal ions in the high-purity thiourea by ion chromatography as claimed in claim 2 or 3, characterized in that the suppressor current is set according to the concentration of the leacheate, wherein the concentration of the leacheate is in mmol/L and the current is in mA, and is set according to three times of the numerical value of the concentration of the leacheate.
5. The method for detecting the content of the trace metal ions in the high-purity thiourea by the ion chromatography as claimed in claim 1, wherein the standard mixed solution in the step 1) and the sample solution in the step 2) are filtered by using an organic RP (RP) small column before being injected.
6. The method for detecting the content of the trace metal ions in the high-purity thiourea by the ion chromatography as claimed in claim 1, wherein the sample solution is filtered by a filter membrane of 0.22 μm before use.
7. The method for detecting the content of the trace metal ions in the high-purity thiourea according to claim 1, wherein the first-stage water is used for removing carbon dioxide and has a conductivity of less than or equal to 0.05 mS/m.
8. The method for detecting the content of the trace metal ions in the high-purity thiourea by the ion chromatography as claimed in claim 1, wherein the ion chromatography system is adopted, and the method comprises the following steps: the protection column is CG12A protection column with size of 4 × 50 mm; the analytical column adopts a CS12A cation exchange column with the size of 4 multiplied by 250 mm; the suppressor model is CERS500, size 4 mm.
9. The method for detecting the content of the trace metal ions in the high-purity thiourea by the ion chromatography as claimed in claim 1, wherein the specific standard mixed solution can be prepared by the following method: taking 10ml of sodium, ammonium, potassium, magnesium and calcium ion standard solutions of 1000ppm respectively, diluting to 100ml with water, preparing 100ppm standard mixed solution, and then preparing 0.01ppm, 0.05ppm, 0.1ppm, 0.2ppm, 0.5ppm, 1ppm, 2ppm and 5ppm standard mixed solution respectively.
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| CN113640398A (en) * | 2021-06-24 | 2021-11-12 | 广东一方制药有限公司 | Method for constructing gypsum standard decoction characteristic map |
| CN115266998A (en) * | 2022-08-03 | 2022-11-01 | 成都普康唯新生物科技有限公司 | Method for detecting content of sodium ions in sodium salt molecules |
| CN115327022A (en) * | 2022-09-13 | 2022-11-11 | 安徽皖维高新材料股份有限公司 | Method for detecting potassium acetate content in PVB resin by adopting ion chromatography |
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| CN113325118A (en) * | 2021-07-21 | 2021-08-31 | 海南通用三洋药业有限公司 | Method for measuring sodium content in parecoxib sodium |
| CN115266998A (en) * | 2022-08-03 | 2022-11-01 | 成都普康唯新生物科技有限公司 | Method for detecting content of sodium ions in sodium salt molecules |
| CN115327022A (en) * | 2022-09-13 | 2022-11-11 | 安徽皖维高新材料股份有限公司 | Method for detecting potassium acetate content in PVB resin by adopting ion chromatography |
| CN115327022B (en) * | 2022-09-13 | 2023-10-24 | 安徽皖维高新材料股份有限公司 | Method for detecting potassium acetate content in PVB resin by adopting ion chromatography |
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