CN210604524U - Detection system for trace bromide ions in sodium persulfate - Google Patents
Detection system for trace bromide ions in sodium persulfate Download PDFInfo
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- CN210604524U CN210604524U CN201921233289.6U CN201921233289U CN210604524U CN 210604524 U CN210604524 U CN 210604524U CN 201921233289 U CN201921233289 U CN 201921233289U CN 210604524 U CN210604524 U CN 210604524U
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Abstract
The utility model discloses a detection system for trace bromide ions in sodium persulfate, which comprises a pre-separation system and a detection system; the pre-separation system comprises a sample injection valve, a pre-separation chromatographic column and a first anion suppressor; the detection system comprises a switching valve, an enrichment column, an analytical chromatographic column and a detector, wherein a sodium persulfate reagent enters the pre-separation chromatographic column through a sample injection valve, and the detection method comprises the pre-separation, enrichment, analysis and regeneration processes. The detection system and the detection method are used for detecting bromide ions in the sodium persulfate, the detection limit of a detected object can be improved, quick pre-separation, high concentration and high-precision detection are realized through switching of the double systems, the detection method is quick, effective and high in accuracy, is suitable for quality control in the production process of the sodium persulfate, and meets the detection requirement of the fine chemical industry.
Description
Technical Field
The utility model relates to an analytical chemistry technique, in particular to a detection system for trace bromide ions in sodium persulfate.
Background
Sodium persulfate, also known as sodium persulfate, is a white crystalline powder in appearance, is odorless, is water soluble, and is useful as a bleaching agent, an oxidizing agent, and an emulsion polymerization accelerator. The existence of trace impurity bromide ions in the sodium persulfate product can affect the performance of the product and the safety of production equipment. Therefore, the method becomes an important link for detecting the trace bromide ions in the production process of the high-purity reagent sodium persulfate. The traditional chemical analysis method is very easy to be interfered by other ions, so that the content determination of the bromide ions can generate huge errors, and the detection speed is relatively slow.
SUMMERY OF THE UTILITY MODEL
In order to solve the deficiencies in the prior art, the utility model aims to provide a detecting system of trace bromide ion in sodium persulfate, use this detecting system to detect the bromide ion in the sodium persulfate, can improve the detection limit of testee, and switching through dual system has realized quick preseparation in addition, high concentration and high accuracy detect, this detection method is swift effective, the degree of accuracy is high, be applicable to the quality control in the sodium persulfate production process, satisfy the detection demand of fine chemistry industry.
The utility model provides a technical scheme that its technical problem adopted does: a detection system for trace bromide ions in sodium persulfate comprises a pre-separation system and a detection system, wherein the pre-separation system is connected with the detection system;
the pre-separation system comprises a sample injection valve, a pre-separation chromatographic column and a first anion suppressor, one end of the pre-separation chromatographic column is connected with the sample injection valve, and the pre-separation chromatographic column is also connected with the detection system through the first anion suppressor;
the detection system comprises a switching valve, an enrichment column, an analytical chromatographic column and a detector, wherein the first anion suppressor and the enrichment column are respectively connected with the switching valve, and the enrichment column is also connected with the detector through the analytical chromatographic column;
and the sodium persulfate reagent enters the pre-separation chromatographic column through a sample injection valve.
Optionally, when the sample injection valve separates the pre-separation chromatographic column, the sample injection valve is connected with the separation eluent and provides the separation eluent for the pre-separation chromatographic column.
Optionally, when the sample injection valve detects bromide ions by the detection system, the sample injection valve is connected with the regeneration eluent and provides the regeneration eluent for the pre-separation chromatographic column.
Optionally, when the switching valve elutes bromide ions in the enrichment column, the switching valve is connected to the analysis eluent and provides the analysis eluent to the enrichment column.
Optionally, the detector comprises a second anion suppressor and a conductivity detector, and the analytical chromatographic column is connected to the conductivity detector through the second anion suppressor.
Adopt above-mentioned technical scheme, the utility model discloses when detecting trace bromide ion in the sodium persulfate, solved the great detection error of traditional chemistry method, also solved the high concentration ion interference and the long drawback of cleaning time of direct adoption ion chromatography testing process, be applicable to the quality control in the sodium persulfate production process, satisfy the detection demand of meticulous chemical industry.
Drawings
Fig. 1 is a state diagram of a detection system of the present invention;
fig. 2 is a state diagram ii of the detection system of the present invention;
fig. 3 is a state diagram of the detection system of the present invention;
FIG. 4 is an analytical chromatogram of prior art bromide ion and other conventional 6 anion standards;
fig. 5 is a chromatogram for analysis of bromide ions in the present invention.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and are not limiting of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in FIGS. 1-3, the utility model discloses a detecting system of trace bromide ion in sodium persulfate, including preseparation system 1 and detecting system 2 in advance, wherein, preseparation system 1 is connected with detecting system 2 in advance to make sodium persulfate reagent switch separately through preseparation system 1 and detecting system 2 and realized quick preseparation, highly concentrated and high accuracy detect, and are swift effective, and the degree of accuracy is high, is applicable to the quality control in the sodium persulfate production process, satisfies the detection demand of fine chemistry industry.
The pre-separation system 1 comprises a sample injection valve 101, a pre-separation chromatographic column 102 and a first anion suppressor 103, wherein one end of the pre-separation chromatographic column 102 is connected with the sample injection valve 101, and the pre-separation chromatographic column 102 is also connected with the detection system 2 through the first anion suppressor 103.
The detection system 2 comprises a switching valve 201, an enrichment column 202, an analytical chromatographic column 203 and a detector 204, wherein the first anion suppressor 103 and the enrichment column 202 are respectively connected with the switching valve 201, and the enrichment column 202 is further connected with the detector 204 through the analytical chromatographic column 203.
The sample valve 101 and the switching valve 201 may adopt a six-way switching valve in a chromatograph autosampler, and the specific structure of the sample valve 101 and the switching valve 201 may refer to the switching valve structure in the liquid chromatograph autosampler, which is not described herein again.
The detector 204 comprises a second anion suppressor 205 and a conductance detector 206, and the analytical chromatography column 203 is connected to the conductance detector 206 via the second anion suppressor 205.
According to the detecting system of trace bromide ion in foretell sodium persulfate, the utility model also provides a detecting method of trace bromide ion in sodium persulfate, including following step:
s1, preparing a pre-separation eluent, a regeneration eluent and an analysis eluent;
s2, conveying a sodium persulfate reagent to a pre-separation chromatographic column 102 through a sample injection valve 101 in the pre-separation system 1;
s3, providing a separation eluent into the pre-separation chromatographic column 102, eluting bromide ions in the sodium persulfate reagent from the pre-separation chromatographic column 102 through the separation eluent and the pre-separation chromatographic column 102, forming a bromide ion aqueous solution through the action of the first anion suppressor 103, and enabling the bromide ion aqueous solution to enter the detection system 2;
s4, in the detection system 2, the switching valve 201 is used to deliver the separated bromide ion aqueous solution to the enrichment column 202, so that the bromide ions are concentrated in the enrichment column 202;
s5, in the detection system 2, supplying an analytical eluent to the enrichment column 202 through the switching valve 201, eluting bromide ions from the enrichment column 202, and transporting to the analytical chromatographic column 203;
s6, the analytical eluent containing bromide ions is separated by the analytical column 203, and then detected by the detector 204.
The detection method of the present invention will be described below with reference to example 1.
Example 1
1. The chromatographic conditions of the pre-separation system 1 were as follows:
(1) pre-separation of leacheate: 16mmol/L potassium hydroxide solution. Accurately weighing 1.7952g of electronic-grade potassium hydroxide in a 2L volumetric flask, using a deionized water solvent, fixing the volume to a scale, and performing suction filtration for later use;
(2) regenerating the leacheate: 100mmol/L sodium potassium hydroxide solution. Precisely weighing 11.22g of electronic-grade potassium hydroxide in a 2L volumetric flask, using a deionized water solvent, fixing the volume to a scale, and performing suction filtration for later use;
(3) flow rate: 1.0 mL/min;
(4) column temperature: 40 ℃;
(5) suppression current of anion suppressor: 50 mA;
(6) pre-separating chromatographic column: HS-5A 4.6X 250mm hydroxide system ion chromatographic column;
(7) automatic injector working pump: a binary low pressure gradient pump.
2. The chromatographic conditions of the detection system 2 were as follows:
(1) analysis of the leacheate: 3.6mmol/L sodium carbonate solution. Accurately weighing 0.7631g of reference grade sodium carbonate in a 2L volumetric flask, using a deionized water solvent, fixing the volume to a scale, and performing suction filtration for later use;
(2) flow rate: 0.8 mL/min;
(3) column temperature: 45 ℃;
(4) suppression current of anion suppressor: 40 mA;
(5) analyzing a chromatographic column: shodex IC SI-524E 4.0 × 250mm carbonate ion chromatographic column;
(6) enriching columns: an ion chromatography trapping column;
(7) automatic injector working pump: a constant-pressure pump.
3. Sample preparation of sodium persulfate:
a sodium persulfate sample 5g is weighed and transferred to a 100mL volumetric flask, dissolved in deionized water and brought to volume to the mark. And (3) taking the diluted sample, filtering the sample by a nylon filter head with the diameter of 0.45 mu m, and then performing machine detection.
4. Carrying out the process
(1) Pre-separation: as shown in fig. 1, a potassium hydroxide solution of 16mmol/L is used as a pre-separation eluent balance pre-separation system 1, 50 μ L of a prepared sample is injected into the pre-separation system 1, a trace amount of bromide ions are washed out of a pre-separation chromatographic column 102 under the action of the pre-separation eluent and the pre-separation chromatographic column 102, a flow path of the pre-separation chromatographic column 102 is cut off by a six-way switching valve of the pre-separation system 1 after all bromide ions are eluted (the total elution time is 20-25 minutes), meanwhile, the pre-separation eluent carries bromide ions to enter a first anion suppressor 103, the pre-separation eluent is converted into an aqueous solution containing bromide ions, and the pre-separation of the trace amount of bromide ions and excessive persulfate is realized;
(2) enrichment: as shown in fig. 2, the bromine ions pumped by the pre-separation system 1 pass through the first anion suppressor 103 to convert the potassium hydroxide solution in the pre-separation eluate into an aqueous solution, and since the water has almost no elution capacity, the bromine ions are kept in the aqueous solution and concentrated by the enrichment column 202 of the detection system 2, and the concentration duration is 2 minutes;
(3) and (3) analysis: as shown in fig. 3, after 2 minutes of enrichment, 3.6mmol/L of sodium carbonate eluent in the detection system 2 is switched to the enrichment column 202, and bromide ions concentrated in the enrichment column 202 are eluted to the carbonate system analytical chromatographic column 203, so that the analysis and detection of bromide ions are realized;
(4) regeneration: as shown in fig. 3, when the detection system 2 enters the analysis stage, the eluent of the pre-separation system 1 is switched to the high-concentration regeneration eluent to elute the sample ions remaining in the pre-separation chromatographic column 102, and after this step, the pre-separation system 1 is switched to the pre-separation eluent, and the pre-separation chromatographic column 102 is switched back to the main flow path by the six-way switching valve, thereby completing the whole regeneration process.
The whole process is circulated in a reciprocating way, so that the continuous detection of trace bromide ions in the high-concentration sodium persulfate can be realized quickly and efficiently.
As shown in figures 4 and 5, through contrast discovery, use the utility model discloses a detection method detects trace bromide ion in to sodium persulfate, can avoid other conventional elements to bromide ion's influence, has solved the great detection error of traditional chemistry method, has also solved the high concentration ion interference that directly adopts the ion chromatography testing process and the long drawback of cleaning time, is applicable to the quality control in the sodium persulfate production process, satisfies the detection demand of meticulous chemical industry.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be understood by those skilled in the art that the scope of the present invention is not limited to the specific combination of the above-mentioned features, but also covers other embodiments formed by any combination of the above-mentioned features or their equivalents without departing from the spirit of the present invention. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Besides the technical features described in the specification, other technical features are known to those skilled in the art, and further description of the other technical features is omitted here in order to highlight the innovative features of the present invention.
Claims (5)
1. The detection system for trace bromide ions in sodium persulfate is characterized by comprising a pre-separation system and a detection system, wherein the pre-separation system is connected with the detection system;
the pre-separation system comprises a sample injection valve, a pre-separation chromatographic column and a first anion suppressor, one end of the pre-separation chromatographic column is connected with the sample injection valve, and the pre-separation chromatographic column is also connected with the detection system through the first anion suppressor;
the detection system comprises a switching valve, an enrichment column, an analytical chromatographic column and a detector, wherein the first anion suppressor and the enrichment column are respectively connected with the switching valve, and the enrichment column is also connected with the detector through the analytical chromatographic column;
and the sodium persulfate reagent enters the pre-separation chromatographic column through the sample injection valve.
2. The system for detecting trace bromide ions in sodium persulfate as claimed in claim 1, wherein the sample injection valve is connected with the separation eluent and supplies the separation eluent to the pre-separation chromatographic column when the pre-separation chromatographic column is used for separation.
3. The detection system for detecting trace bromide ions in sodium persulfate according to claim 2, wherein when the detection system detects bromide ions, the sample injection valve is connected with the regeneration eluent and supplies the regeneration eluent to the pre-separation chromatographic column.
4. The system for detecting trace amounts of bromide ions in sodium persulfate as set forth in claim 3, wherein the switching valve is connected to the analytical eluent and supplies the analytical eluent to the enrichment column when the switching valve is used for eluting bromide ions in the enrichment column.
5. The system for detecting sodium persulfate medium-trace bromide ions according to claim 1, wherein the detector comprises a second anion suppressor and a conductivity detector, and the analytical chromatographic column is connected with the conductivity detector through the second anion suppressor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110412161A (en) * | 2019-07-31 | 2019-11-05 | 安徽皖仪科技股份有限公司 | The detection system and detection method of micro bromide ion in a kind of sodium peroxydisulfate |
| CN114910575A (en) * | 2022-04-07 | 2022-08-16 | 浙江西热利华智能传感技术有限公司 | Power station water vapor anion analysis system and method based on chromatography |
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2019
- 2019-07-31 CN CN201921233289.6U patent/CN210604524U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110412161A (en) * | 2019-07-31 | 2019-11-05 | 安徽皖仪科技股份有限公司 | The detection system and detection method of micro bromide ion in a kind of sodium peroxydisulfate |
| CN114910575A (en) * | 2022-04-07 | 2022-08-16 | 浙江西热利华智能传感技术有限公司 | Power station water vapor anion analysis system and method based on chromatography |
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