CN114660223A - Low-background ultra-trace ion detection device and method - Google Patents
Low-background ultra-trace ion detection device and method Download PDFInfo
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- CN114660223A CN114660223A CN202210455424.1A CN202210455424A CN114660223A CN 114660223 A CN114660223 A CN 114660223A CN 202210455424 A CN202210455424 A CN 202210455424A CN 114660223 A CN114660223 A CN 114660223A
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Abstract
The invention belongs to the technical field of analytical chemistry, and discloses a low-background ultra-trace ion detection device and a method, wherein the device comprises an air filtering system and a detection system, the air filtering system comprises a compressed air source, a first absorption bottle, a second absorption bottle, a third absorption bottle and a safety bottle, and the detection system comprises a glove box, a large-volume automatic sample injector and an ion chromatograph; the gas filtering system and the detection system are connected with the glove box through the safety bottle, the large-volume automatic sample injector is arranged in the glove box, and the detection method is further disclosed.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a low-background ultra-trace ion detection device and method. Background
The air contains a lot of ions, the sample is easy to absorb other ions in the air before sample injection, the result in the detection process is higher than the actual result, the detection influence on the ions in the low-content sample is larger, the solution to the problem in the prior art is to cover a sample injection bottle, the contact area between the sample and the air is reduced, but the sample cannot be completely prevented from being polluted, the effect is very little and the cost is increased.
Disclosure of Invention
Based on this, it is necessary to provide an ultra trace ion detection device with low background to solve the technical problem of air ion interference at present, and the device has great significance to the technical field of analytical chemistry.
The invention aims to provide a low-background ultra trace ion detection device, which specifically comprises:
the device comprises an air filtering system and a detection system, wherein the air filtering system comprises a compressed air source, a first absorption bottle, a second absorption bottle, a third absorption bottle and a safety bottle, and the detection system comprises a glove box, a large-volume automatic sample injector and an ion chromatograph; the gas filtering system and the detection system are connected with the glove box through a safety bottle, and the large-volume automatic sample injector is arranged inside the glove box;
the ultra-trace ion detection device with the low background specifically comprises a compressed air source connected with a first absorption bottle, a first absorption bottle connected with a second absorption bottle, a second absorption bottle connected with a third absorption bottle, a third absorption bottle connected with a safety bottle, a safety bottle connected with a glove box, a large-volume automatic sample injector arranged in the glove box, and a large-volume automatic sample injector connected with an ion chromatograph.
Preferably, the solution in the first absorption bottle is a sodium hydroxide solution with the concentration of 1 mmol/L-5 mol/L, and is a potassium hydroxide solution with the concentration of 1 mmol/L-5 mol/L.
Preferably, the solution in the second absorption bottle is phosphoric acid solution with the concentration of 1 mmol/L-5 mol/L, and sulfuric acid with the concentration of 1 mmol/L-5 mol/L is selected for the second time.
Preferably, the solution in the third absorption bottle is ultrapure water.
Preferably, the safety bottle does not contain a solution.
Preferably, the glove box body is provided with a glove box, a safety bottle connector and a glove box exhaust port.
Preferably, the sample injection volume of the large-volume autosampler ranges from 1mL to 100 mL.
Preferably, the materials of the first absorption bottle, the second absorption bottle, the third absorption bottle and the safety bottle are preferably polytetrafluoroethylene, and polypropylene is selected as a second choice.
Another purpose is to provide a low background ultra trace ion detection method, the specific technical scheme is as follows:
s1, manufacturing a high-purity sample injection environment: pumping air into a first absorption bottle by a compressed air source to remove acid gas; then removing alkaline gas in a second absorption bottle, removing impurities possibly existing in the gas in a third absorption bottle, then entering a safety bottle for buffer drying, and finally entering the pretreated gas into a glove box;
s2, placing the sample on a large-volume automatic sample injector in a glove box, and carrying out large-volume sample injection;
and S3, the sample enters an ion chromatograph along with the mobile phase for detection.
Compared with the existing scheme, the low-background ultra-trace ion detection device and method have the following beneficial effects: the invention makes a low blank sample introduction atmosphere without ion interference through the gas filtering system, improves the sensitivity and the accuracy through large-volume sample introduction, reduces the blank background by the device combining method, improves the sensitivity of the instrument, reduces the interference of detection, and has the advantages of simple structure, easy operation and low operation cost.
Drawings
FIG. 1 is a block diagram of a low background ultra trace ion detection device;
FIG. 2 is a diagram of the detection of 0.5ppb anion (F) using a low background ultra trace ion detection device-、Cl-、Br-、NO2 -、NO3 -、SO4 2-、PO4 2-) A chromatogram of the standard solution;
FIG. 3 is a diagram of the detection of 0.5ppb cation (Li) using a low background ultra trace ion detection device in combination with a detection method+、Na+、NH4 +、K+、Mg2+、Ca2+) A chromatogram of the standard solution;
FIG. 4 is a chromatogram for detecting anions in high purity water using a low background ultra trace ion detection device;
FIG. 5 is a chromatogram for detecting cations in high purity water using a low background ultra trace ion detection device.
Detailed Description
Wherein in FIG. 1, 1-compressed air source; 2-a first absorption bottle; 3-a second absorption bottle; 4-a third absorption bottle; 5-a safety bottle; 6-connecting the glove box with a safety bottle; 7-glove box vent; 8-glove box; 9-a large volume autosampler; 10-ion chromatograph.
Example 1
The invention provides a low-background ultra-trace ion detection method, which specifically comprises the following steps:
s1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
and S3, the sample enters the ion chromatograph (10) along with the mobile phase for detection.
Example 2
As shown in fig. 1, the present invention provides a low background ultra trace ion detection apparatus, which specifically includes:
the device comprises an air filtering system and a detection system, wherein the air filtering system comprises a compressed air source (1), a first absorption bottle (2), a second absorption bottle (3), a third absorption bottle (4) and a safety bottle (5), and the detection system comprises a glove box (8), a large-volume automatic sample injector (9) and an ion chromatograph (10); the air filtering system and the detection system are connected with a glove box (8) through a safety bottle (5), and a large-volume automatic sample injector (9) is arranged inside the glove box.
The ultra-trace ion detection device with the low background comprises a compressed air source, a first absorption bottle (2), a second absorption bottle (3), a third absorption bottle (4), a safety bottle (5), a glove box (8), a large-volume automatic sample injector (9), and an ion chromatograph (10), wherein the first absorption bottle (2) is connected with the compressed air source, the second absorption bottle (2) is connected with the second absorption bottle (3), the third absorption bottle (4) is connected with the third absorption bottle (4), the safety bottle (5) is connected with the glove box (8), the large-volume automatic sample injector (9) is arranged in the glove box (8), and the large-volume automatic sample injector (9) is connected with the ion chromatograph (10).
The solution in the first absorption bottle (2) is preferably a potassium hydroxide solution with the concentration of 1 mmol/L-5 mol/L, and is selected as a potassium hydroxide solution with the concentration of 1 mmol/L-5 mol/L;
the solution in the second absorption bottle (3) is preferably a sulfuric acid solution with the concentration of 1 mmol/L-5 mol/L, and is selected as sulfuric acid for the second time with the concentration of 1 mmol/L-5 mol/L;
the solution in the third absorption bottle (4) is ultrapure water;
no solution is placed in the safety bottle (5);
the box body of the glove box (8) is provided with a port (6) for connecting the glove box and the safety bottle and an exhaust port (7) for the glove box;
the sample injection volume range of the large-volume automatic sample injector is 1-100 mL;
the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are preferably made of polytetrafluoroethylene, and polypropylene is selected in a second time.
Example 3
Low-background ultra-trace ion detection device combined detection method for detecting 0.5ppb anions (F)-、Cl-、Br-、NO2 -、NO3 -、SO4 2-、PO4 2-) Standard solutions, conditions were as follows:
the solution in the first absorption bottle (2) is sodium hydroxide solution, and the concentration is 1 mmol/L;
the solution in the second absorption bottle (3) is phosphoric acid solution, and the concentration is 1 mmol/L;
the solution in the third absorption bottle (4) is ultrapure water;
no solution is in the safety bottle (5);
the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are made of polytetrafluoroethylene.
Detailed description of the preferred embodiment
S1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
s3, the sample enters the ion chromatograph (10) along with the mobile phase for detection, and the working conditions of the ion chromatograph are set as follows:
a chromatographic column: dionex IonPacTMAS11-HC
Leacheate: 0-8min, 5mmol/LKOH, 8-20min, 20 mmol/LKOH; 20-23 min, 20 mmol/LKOH; 23-24min, 40 mmol/LKOH; 24-29min, 40 mmol/LKOH; 29-31min, 5mmol/LKOH
Flow rate of eluent: 1.0mL/min
The temperature of the pool is as follows: 40 deg.C
Column temperature: 40 deg.C
Sample introduction amount: 2mL
Then, the automatic analysis of the instrument was started, and the measurement results are shown in FIG. 2.
Example 4
Low-background ultra-trace ion detection device combined detection method for detecting 0.5ppb cations (Li)+、Na+、NH4 +、K+、Mg2+、Ca2+) Standard solutions, conditions were as follows:
the solution in the first absorption bottle (2) is sodium hydroxide solution, and the concentration is 1 mmol/L;
the solution in the second absorption bottle (3) is phosphoric acid solution, and the concentration is 1 mmol/L;
the solution in the third absorption bottle (4) is ultrapure water;
no solution is in the safety bottle (5);
the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are made of polytetrafluoroethylene.
Detailed description of the preferred embodiment
S1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
s3, the sample enters the ion chromatograph (10) along with the mobile phase for detection, and the working conditions of the ion chromatograph are set as follows:
and (3) chromatographic column: dionex IonPacTMCS16
Leacheate: 30mmol/L methanesulfonic acid
Flow rate of eluent: 1.0mL/min
The temperature of the pool is: 40 deg.C
Column temperature: 40 deg.C
Sample introduction amount: 2mL
The automatic analysis of the instrument was then started and the results are shown in FIG. 3.
Example 5
A low-background ultra-trace ion detection device is combined with a detection method to detect anions in high-purity water, and the conditions are as follows:
the solution in the first absorption bottle (2) is sodium hydroxide solution, and the concentration is 2.5 mol/L;
the solution in the second absorption bottle (3) is phosphoric acid solution, and the concentration is 2.5 mol/L;
the solution in the third absorption bottle (4) is ultrapure water;
no solution is in the safety bottle (5);
the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are made of polypropylene.
Detailed description of the preferred embodiment
S1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
s3, the sample enters the ion chromatograph (10) along with the mobile phase for detection, and the working conditions of the ion chromatograph are set as follows:
a chromatographic column: dionex IonPacTMAS11-HC
Leacheate: 0-8min, 5mmol/LKOH, 8-20min, 20 mmol/LKOH; 20-23 min, 20 mmol/LKOH; 23-24min, 40 mmol/LKOH; 24-29min, 40 mmol/LKOH; 29-31min, 5mmol/LKOH
Flow rate of eluent: 1.0mL/min
The temperature of the pool is: 40 deg.C
Column temperature: 40 deg.C
Sample introduction amount: 2mL
The automatic analysis of the instrument was then started and the results are shown in FIG. 4.
Example 6
A low-background ultra-trace ion detection device is combined with a detection method to detect cations in high-purity water, and the conditions are as follows:
the solution in the first absorption bottle (2) is sodium hydroxide solution, and the concentration is 5 mol/L;
the solution in the second absorption bottle (3) is phosphoric acid solution, and the concentration is 5 mol/L;
the solution in the third absorption bottle (4) is ultrapure water;
the safety bottle (5) has no solution;
the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are made of polypropylene.
Detailed description of the preferred embodiment
S1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
s3, the sample enters the ion chromatograph (10) along with the mobile phase for detection, and the working conditions of the ion chromatograph are set as follows:
and (3) chromatographic column: dionex IonPacTMCS16
Leacheate: 30mmol/L methanesulfonic acid
Flow rate of eluent: 1.0mL/min
The temperature of the pool is as follows: 40 deg.C
Column temperature: 40 deg.C
Sample introduction amount: 2mL
The automatic analysis of the instrument was then started and the results are shown in FIG. 5.
The present invention is described above with reference to specific examples. It should be noted that the above embodiments are only used for further illustration of the present invention, and do not represent the scope of the present invention, and that other non-essential modifications and adjustments made according to the teachings of the present invention still belong to the scope of the present invention.
Claims (9)
1. The ultra trace ion detection device and the method with the low background are characterized by comprising an air filtering system and a detection system, wherein the air filtering system comprises a compressed air source (1), a first absorption bottle (2), a second absorption bottle (3), a third absorption bottle (4) and a safety bottle (5), the detection system comprises a glove box (8), a large-volume automatic sample injector (9) and an ion chromatograph (10), the air filtering system and the detection system are connected with the glove box (8) through the safety bottle (5), and the large-volume automatic sample injector (9) is arranged inside the glove box;
the ultra-trace ion detection device with the low background specifically comprises a compressed air source (1) connected with a first absorption bottle (2), the first absorption bottle (2) connected with a second absorption bottle (3), the second absorption bottle (3) connected with a third absorption bottle (4), the third absorption bottle (4) connected with a safety bottle (5), the safety bottle (5) connected with a glove box (8), a large-volume automatic sample injector (9) arranged inside the glove box (8), and the large-volume automatic sample injector (9) connected with an ion chromatograph (10).
2. The low-background ultra trace ion detection device according to claim 1, wherein the solution in the first absorption bottle (2) is preferably a sodium hydroxide solution with a concentration of 1 mmol/L-5 mol/L, and is preferably a potassium hydroxide solution with a concentration of 1 mmol/L-5 mol/L.
3. The low-background ultra trace ion detection device according to claim 1, wherein the solution in the second absorption bottle (3) is preferably phosphoric acid solution with a concentration of 1 mmol/L-5 mol/L, and is sulfuric acid with a concentration of 1 mmol/L-5 mol/L in a second selection.
4. The low background ultra trace ion detection device according to claim 1, wherein the solution in the third absorption bottle (4) is ultra pure water.
5. A low background ultra trace ion detection device according to claim 1, wherein no solution is placed in the safety bottle (5).
6. The low background ultra trace ion detection device according to claim 1, wherein the glove box (8) housing is provided with a glove box and safety bottle interface (6) and a glove box vent (7).
7. The low-background ultra trace ion detection device according to claim 1, wherein the sample injection volume of the large-volume autosampler is in a range of 1 mL-100 mL.
8. The low background ultra trace ion detection device according to claim 1, wherein the first absorption bottle (2), the second absorption bottle (3), the third absorption bottle (4) and the safety bottle (5) are made of polytetrafluoroethylene, and polypropylene is selected as the second choice.
9. A low background ultra trace ion detection method is characterized in that,
s1, manufacturing a high-purity sample injection environment: a compressed air source (1) pumps air into a first absorption bottle (2) to remove acid gas; then removing alkaline gas in a second absorption bottle (3), removing impurities possibly existing in the gas in a third absorption bottle (4), then entering a safety bottle (5) for buffer drying, and finally entering the pretreated gas into a glove box (8);
s2, placing the sample on a large-volume automatic sample injector (9) in a glove box (8) for large-volume sample injection;
and S3, the sample enters the ion chromatograph (10) along with the mobile phase for detection.
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| CN202210455424.1A CN114660223A (en) | 2022-04-28 | 2022-04-28 | Low-background ultra-trace ion detection device and method |
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