# US 2021/0364435 A1 · Atomic fluorescence analysis method and device using water as carrier fluid

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- Number: US 2021/0364435 A1
- Document ID: US20210364435A1
- Status: Published application
- Kind: A1
- Application number: 17/286,617
- Filed: 2019-04-25
- Published: 2021-11-25
- Earliest claimed: 2018-10-29
- Assignees: Chongqing Mintai New Agrotech Development Group C., Ltd.
- Applicants: Chongqing Mintai New Agrotech Development Group C., Ltd.
- Inventors: Mei YANG; Zhixiang GONG; Hui GONG
- Web page: https://patentgrep.com/patent/US20210364435A1

## CPC

- G01N 21/6404: {Atomic fluorescence}
- G01N 1/14: Suction devices, e.g. pumps; Ejector devices
- G01N 2001/1463: {Injector; Air-lift}
- G01N 2001/149: {Capillaries; Sponges}
- G01N 2021/6406: {multi-element}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The invention discloses an atomic fluorescence analysis method and device using water as a carrier fluid, belonging to the atomic fluorescence analysis in the field of analytical chemistry; the method is to replace hydrochloric acid and a reducing agent with water as the carrier fluid in the conventional sampling and fluid delivery process to carry the test liquid and reagent into the reactor to complete a reaction. The invention effectively overcomes the memory effect by using water as the carrier fluid and improves the determination sensitivity and accuracy, which saves a large amount of high-purity hydrochloric acid and reducing agent at the same time, greatly reducing the analysis cost, and significantly improving the operating environment, which is the innovation of atomic fluorescence analysis technology.

## Claims

### Claim 1

An atomic fluorescence analysis method using water as a carrier fluid, comprising: sampling and fluid delivery, making a test solution and a reagent to react in a reactor, atomizing element to be tested and determining fluorescence, wherein, in the conventional sampling and fluid delivery process, water is used as the carrier fluid, so that the test solution and the reagent are carried into the reactor by water to complete the reaction, wherein the reagent is reducing agent.

### Claim 2 (depends on 1)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 1, wherein the sampling and fluid delivery process is sampling first and then fluid delivery, the sampling first being to introduce the test solution with a certain acidity and the reagent with a certain concentration, respectively, and the then fluid delivery being to use pure water as the carrier fluid to carry the test solution and reagent into the reactor.

### Claim 3 (depends on 2)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 2, wherein the sampling time is 4-5 seconds, and the time from the fluid delivery to completion of the determination is 8-10 seconds.

### Claim 4 (depends on 3)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 3, the acidity of the test solution is related to the element to be tested, wherein the acidity of the test solution is adjusted by hydrochloric acid, the concentration range of hydrochloric acid in the test solution is from 4%-10%, and the relationship between the concentration and the acidity of the common elements to be tested is as shown in Table 1.

### Claim 5

An atomic fluorescence analysis device using water as a carrier fluid, comprising: a fluid delivery system, a reactor, an atomizer, an excitation light source, and a detector, wherein the fluid delivery system including:
a test solution bottle for containing the sample solution to be tested, which is connected to the reactor through a sample inlet tube;
a reagent bottle for containing the reducing agent, which is connected to the reactor through a reagent inlet tube;
a water bottle for containing pure water, with the water bottle outlets of which connected to the inlet of the sample inlet tube and the inlet of the reagent inlet tube through two water inlet tubes, and a switch is configured to control the water intake from the water inlet tube to the sample inlet tube or the reagent inlet tube; and
the fluid delivery system does not contain a supporting device for delivering and injecting the carrier acid.

### Claim 6 (depends on 5)

The atomic fluorescence analysis device using water as a carrier fluid according to claim 5, wherein the sample inlet tube and the reagent inlet tube are both liquid inlet capillary tubes, and the water bottle is changed into two water cups, one of the water cups used for water for cleaning, the other used for water for carrier fluid, and the liquid inlet head ends of the two liquid inlet capillary tubes are able to be alternately inserted into the two glasses of water.

### Claim 7 (depends on 6)

The atomic fluorescence analysis device using water as a carrier current according to claim 6, wherein the two liquid inlet capillary tubes are connected to the reactor through a peristaltic pump, and the peristaltic pump controls the delivery speed and delivery volume of the test solution, reagent and water for carrier fluid in the liquid inlet capillary tubes.

### Claim 8 (depends on 5)

An atomic fluorescence analysis method using water as a carrier fluid, using the device of claim 5, the method comprising:
step 1. preparing a series of standard solutions with different concentrations of the elements to be tested, sample solution and reagent solution, and the sample solution is put into the test solution bottle, the reagent solution is put into the reagent bottle; and the pure water is put into the water bottle;
step 2. making a standard curve:
1) sampling: connecting the sample inlet tube to the inlet of the test solution containing a standard blank solution, and connecting the reagent inlet tube to the inlet of the reagent bottle;
2) fluid delivery: turning on the switch to connect the sample inlet tube and the reagent inlet tube with the water inlet tube to make the pure water in the water bottle enter the sample inlet tube and the reagent inlet tube, and carry and push the standard blank solution and the reagent solution into the reactor respectively;
3) determining: making the reactor, the atomizer and the excitation light source work and obtaining a blank fluorescence value by the detector;
4) replacing the test solution bottles containing the series of standard solutions with different concentrations in the order of concentration from low to high; repeating steps 1)-3), and sequentially determining and obtaining the fluorescence value of each standard solution;
5) drawing a fluorescence value-concentration standard curve;
step 3. sample determination: replacing the test solution bottle containing the sample solution; repeating 1)-3) in step 2 to determine and obtain the corresponding fluorescence value of the sample solution, and obtaining the concentration of the element to be tested in the sample solution via the fluorescence value-concentration standard curve.

### Claim 9 (depends on 8)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 8, wherein the sampling time in step 1) is 4-5 seconds; the time from the fluid delivery in step 2) to obtaining the fluorescence value by the detector in step 3) is 8-10 seconds.

### Claim 10 (depends on 6)

An atomic fluorescence analysis method using water as a carrier fluid, using the device according to claim 6, the method comprising:
operation 1. preparing a series of standard solutions with different concentrations of the elements to be tested, sample solution and reagent solution as required, and preparing two cups of pure water;
operation 2. initiating the atomic fluorometer and adjusting the atomic fluorometer to the required working state;
operation 3. making a standard curve:
A1) sampling: inserting the liquid inlet ends of the two liquid inlet capillary tubes into a standard blank solution and the reagent solution for sampling respectively, and after 4-5 seconds stopping the peristaltic pump;
A2) replacing insertion: taking out the liquid inlet ends of the two liquid inlet capillary tubes and placing them in a cup of cleaning water for cleaning, and then transferring them to the water for carrier fluid in the other cup; and re-initiating the peristaltic pump;
A3) carrier fluid determination: carrying the standard blank solution and the reagent solution into the reactor by the carrier fluid, respectively, and obtaining the blank fluorescence value by the detector;
A4) replacing the standard blank solution with the series of standard solutions with different concentrations in the order of concentration from low to high; repeating A1)-A3), and sequentially determining and obtaining the fluorescence value of each standard solution;
A5) drawing a fluorescence value-concentration standard curve; operation 4. sample determination: replacing the standard blank solution with the sample solution; determining and obtaining the fluorescence value of the sample solution according to operations A1)-A3); obtaining the concentration of the element to be tested in the sample solution from the fluorescence value-concentration standard curve, and entering the relevant parameters to calculate the content of the determined element in the sample.

### Claim 11 (depends on 10)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 10, wherein the sampling/delaying/replacing insertion/determination time is 4-5/0/2-3/8-10 seconds, respectively, wherein the delaying is an operation after the sampling, that is, the sampling time in A1) is 4-5 seconds, the delaying time is zero seconds, the replacing insertion time in A2) is 2-3, and the carrier fluid determination time in A3) is 8-10 seconds.

### Claim 12 (depends on 7)

An atomic fluorescence analysis method using water as a carrier fluid, using the device according to claim 7, the method comprising:
operation 1. preparing a series of standard solutions with different concentrations of the elements to be tested, sample solution and reagent solution as required, and preparing two cups of pure water;
operation 2. initiating the atomic fluorometer and adjusting the atomic fluorometer to the required working state;
operation 3. making a standard curve:
A1) sampling: inserting the liquid inlet ends of the two liquid inlet capillary tubes into a standard blank solution and the reagent solution for sampling respectively, and after 4-5 seconds stopping the peristaltic pump;
A2) replacing insertion: taking out the liquid inlet ends of the two liquid inlet capillary tubes and placing them in a cup of cleaning water for cleaning, and then transferring them to the water for carrier fluid in the other cup; and re-initiating the peristaltic pump;
A3) carrier fluid determination: carrying the standard blank solution and the reagent solution into the reactor by the carrier fluid, respectively, and obtaining the blank fluorescence value by the detector;
A4) replacing the standard blank solution with the series of standard solutions with different concentrations in the order of concentration from low to high; repeating A1)-A3), and sequentially determining and obtaining the fluorescence value of each standard solution;
A5) drawing a fluorescence value-concentration standard curve;
operation 4. sample determination: replacing the standard blank solution with the sample solution; determining and obtaining the fluorescence value of the sample solution according to operations A1)-A3); obtaining the concentration of the element to be tested in the sample solution from the fluorescence value-concentration standard curve, and entering the relevant parameters to calculate the content of the determined element in the sample.

### Claim 13 (depends on 12)

The atomic fluorescence analysis method using water as a carrier fluid according to claim 12, wherein the sampling/delaying/replacing insertion/determination time is 4-5/0/2-3/8-10 seconds, respectively, wherein the delaying is an operation after the sampling, that is, the sampling time in A1) is 4-5 seconds, the delaying time is zero seconds, the replacing insertion time in A2) is 2-3, and the carrier fluid determination time in A3) is 8-10 seconds.