CN209821067U - Mercury atom fluorescence tester taking water as current-carrying and liquid conveying system therein - Google Patents
Mercury atom fluorescence tester taking water as current-carrying and liquid conveying system therein Download PDFInfo
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- CN209821067U CN209821067U CN201920115618.0U CN201920115618U CN209821067U CN 209821067 U CN209821067 U CN 209821067U CN 201920115618 U CN201920115618 U CN 201920115618U CN 209821067 U CN209821067 U CN 209821067U
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Abstract
The utility model discloses an use mercury atom fluorescence apparatus of water as current-carrying and infusion system wherein, including infusion system, reactor, atomizer, excitation light source and detector etc. characteristics are that infusion system includes: the device comprises a test solution bottle, a reagent bottle and a water bottle, wherein a water outlet of the water bottle is respectively communicated with a liquid inlet of the test solution bottle and a liquid inlet of the reagent bottle through two water inlet pipes, a change-over switch is arranged on each water inlet pipe, the liquid outlets of the test solution bottle and the reagent bottle are communicated with a reactor, and a matching device for injecting acid liquor for carrying flow is not contained in an infusion system. When the utility model is used for analyzing mercury, water is used as the current carrying, the memory effect in mercury determination can be effectively overcome, the determination sensitivity and accuracy are improved,simultaneously saves a large amount of high-purity HCl and NaBH serving as a reducing agent4The analysis cost is greatly reduced, the operation environment is also obviously improved, and the method is an innovation of the mercury atom fluorescence analysis technology.
Description
Technical Field
The utility model belongs to the analytical chemistry field relates to the atomic fluorescence analytical instrument of mercury. The device breaks through the traditional infusion mode and the corresponding technology in the atomic fluorescence analysis of mercury, and particularly relates to the improvement of the existing mercury atomic fluorescence tester.
Background
Atomic fluorescence analysis has been widely used for the determination of trace amounts of Hg elements. The basic principle is that ions of mercury element in an acidic medium (usually hydrochloric acid) react with a strong reducing agent (usually potassium borohydride or sodium borohydride) to be reduced into mercury atoms, and a large amount of hydrogen is generated. The mercury atoms are excited to a high energy state by radiation of a specific frequency of the excitation light source, and the excited state atoms emit fluorescence of a characteristic wavelength in the form of light radiation during the deexcitation process due to the extreme instability of the high energy level. The fluorescence intensity is correlated with the concentration of mercury, and the concentration of elemental mercury is determined by measuring the fluorescence signal from a detector (usually a photomultiplier tube).
The mercury atom fluorescence tester designed according to the above principle mainly comprises a transfusion system, a vapor generation system (or called as a reactor), an atomizer, an excitation light source and a detection system. The mercury test solution and the reducing agent are conveyed through the liquid conveying system and are carried by carrier liquid (also called carrier liquid) to be sent into the reactor to carry out chemical reaction to generate mercury atom vapor and hydrogen, and the mercury atom vapor and the hydrogen enter the atomizer under the carrying of the carrier gas (usually argon) to be further excited to generate fluorescence for detection.
In the atomic fluorescence analysis of mercury, HCl and NaBH are always used for carrying mercury test solution and reagent4(or KBH4) This technique has the following drawbacks: the transfusion system has serious memory effect, and particularly after a high-concentration mercury sample is measured, a capillary tube for conveying a mercury test solution needs to be cleaned for many times by using blank liquid to measure the next mercury sampleThe time consumption is long due to the fact that samples are used, and even the infusion system needs to be completely replaced; a large amount of acid carrier fluid needs to be continuously used in the infusion process, so that the pollution to the operating environment is brought, a detection instrument is corroded, and meanwhile, a large amount of high-purity HCl and a valuable reduction reagent are consumed in the carrier process, so that the detection cost is increased.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide an use mercury atom fluorescence apparatus of water as current-carrying.
The utility model discloses use water as mercury atom fluorescence apparatus of current-carrying, including infusion system, reactor, atomizer, excitation light source and detector etc. characteristics are: the infusion system comprises a test solution bottle, a reagent bottle and a water bottle, purified water is contained in the water bottle, a water outlet of the water bottle is communicated with inlets of the test solution bottle and the reagent bottle respectively through two water inlet pipes, a change-over switch is arranged on each water inlet pipe, and liquid outlets of the test solution bottle and the reagent bottle are communicated with the reactor respectively.
The mercury test solution bottle is used for containing mercury test solution to be tested and is communicated with the reactor through the sample inlet pipe; the reagent bottle is used for containing a reducing agent and is communicated with the reactor through a reagent inlet pipe; the water bottle is only used for containing pure water; and the infusion system does not contain a matched device for infusing acid liquor for carrying flow.
The sample inlet pipe and the reagent inlet pipe are both liquid inlet capillary pipes.
The mercury atom fluorescence tester taking water as a current-carrying material also comprises a peristaltic pump, wherein liquid inlet capillary tubes of the sample inlet tube and the reagent inlet tube are arranged in the peristaltic pump, and liquid is respectively conveyed into the reactor through the peristaltic pump.
The mercury atom fluorescence tester taking water as current carrying also comprises a sample storage ring, and the extension parts of the sample inlet pipe and the reagent inlet pipe at the rear end of the peristaltic pump are the respective sample storage rings.
The utility model further provides a simplified mercury atom fluorescence tester taking water as current carrying, in the simplified tester, a sample inlet pipe and a reagent inlet pipe of a transfusion system are liquid inlet capillary pipes, one end of each liquid inlet capillary pipe is connected into a reactor, and the other end is a free end and is inserted into the solution of a test solution bottle or a reagent bottle; the water bottle is changed into two water cups, one water cup is used for containing cleaning water, the other water cup is used for containing carrier water, the free end of the liquid inlet capillary tube is a water inlet tube of the water bottle, and the free end of the liquid inlet capillary tube can be replaced and inserted between the two water cups.
The transfusion system specially used in the mercury atom fluorescence tester taking water as current carrying also belongs to the content of the utility model.
Scheme more than adopting, the utility model discloses use water to do not contain the supporting device of infusion acidizing fluid for the carrier flow for mercury atomic fluorescence apparatus of current-carrying, infusion process provides the pure water through water-jug or drinking cup, and through the simple switching of inlet tube or the trade of capillary free end insert, can use water as the current-carrying at the atomic fluorescence analysis process of mercury, has ended for more than 30 years and has used HCl and NaBH4Is the history of the current carrying. The detection examples prove that: the transfusion technology using water to replace HCl and a reducing agent as a current carrier is used for mercury atom fluorescence analysis, not only can trace or trace Hg and the like in a test solution be detected, but also the technical bias that the water cannot be used as the current carrier in the conventional knowledge is overcome; meanwhile, different from the method for measuring mercury by taking HCl and NaBH4 as current carriers, ultrapure water does not contain a component to be measured, does not have any chemical reaction with a test solution or a reducing agent in the process of infusion, does not have a large number of bubbles (caused by hydrogen generated by acid and the reducing agent) adhered to the tube wall of a flow path, and can wash all infusion flow paths thoroughly while carrying current, so that the memory effect in the fluorescence measurement of mercury atoms can be effectively overcome, the measurement sensitivity and accuracy are improved, and the measurement can be carried out even when the Hg concentration is lower than 0.1ng/ml (0.04 ng/ml in example 3); in addition, water is used as a carrier fluid, so that a large amount of high-purity HCl and NaBH serving as a reducing agent for the carrier fluid are saved4The analysis cost is greatly reduced, and the operation environment is also obviously improved.
The present invention will be described in detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1A is a schematic diagram showing the configuration of a two-channel atomic fluorescence analyzer of a combined water-borne flow infusion system;
FIG. 1B is a schematic view of a mercury atomic fluorescence measuring instrument using water as a carrier according to the present invention;
FIG. 2 is a simplified fluid delivery system and fluid delivery schematic diagram for mercury atomic fluorescence analysis using water as a carrier according to the present invention;
FIG. 3 is a graph of Hg measured by the mercury atomic fluorescence measuring apparatus of the present invention using water as carrier in example 1, wherein A is a peak value curve (fluorescence value-time) and B is a standard curve (fluorescence value-concentration) of Hg concentration of 1-5 ng/mL;
FIG. 4 is a graph showing the peak value curve (A, fluorescence value vs. time) of Hg/As and a standard curve (B, fluorescence value vs. concentration) of a mixed solution of 0.2-1.0ng/mL Hg and 10-50ng/mL As measured simultaneously by a two-channel atomic fluorescence analyzer using water As a carrier in example 2;
FIG. 5 is a photograph of example 3, showing Hg in rice measured by a mercury atomic fluorescence measuring apparatus using water as a carrier, wherein A is a screenshot of measured data of a standard solution of Hg, B is a peak value curve (fluorescence value-time), and C is a standard curve (fluorescence value-concentration) of 0.1-0.5 ng/mLHg.
Detailed Description
The utility model provides a mercury atom fluorescence apparatus using water as current-carrying.
Based on the atomic fluorescence analysis technology, a conventional atomic fluorescence analysis apparatus generally includes a liquid delivery system, a reactor, an atomizer, an excitation light source, and a detector (see fig. 1A for the relationship of components, fig. 1A is a two-channel atomic fluorescence analysis apparatus designed by the applicant, which can be used to simultaneously measure Hg and As), and a mercury atomic fluorescence measurement instrument based on the atomic fluorescence analysis principle is basically configured similarly, only the excitation light source is a single mercury hollow cathode lamp (see fig. 1B), wherein a sample liquid and a reducing agent (reagent) are respectively introduced into the reactor from the liquid delivery system, and hydrochloric acid and the reducing agent are respectively used As carrier currents during the introduction.
The utility model discloses a design is at conventional mercury atom fluorescence analysis infusion in-process, utilizes water to replace HCl and reductant (reagent) to do the current-carrying, is inputing test solution and reagent from the imbibition capillary respectively to depositing appearance ring separately after, and two capillaries all do the current-carrying with the pure water, and test solution and reagent in the appearance ring of depositing separately react in being pushed into the reactor under the carrier band of water, and simultaneously, the pure water of current-carrying also washs the pipeline of infusion system.
According to the above design, the utility model discloses use water as the constitution of the mercury atom fluorescence apparatus of current-carrying and see that fig. 1B shows, wherein the infusion system includes: the test solution bottle is used for containing a sample solution to be tested and is communicated with the reactor through a sample inlet pipe; the reagent bottle is used for containing a reducing agent and is communicated with the reactor through a reagent inlet pipe; the water outlet of the water bottle is communicated with the inlet of the sample inlet pipe and the inlet of the reagent inlet pipe respectively through the water inlet pipe, and the water inlet is controlled by switching the water inlet pipe. The infusion system is specially designed, and does not comprise a matching device for infusing the current-carrying hydrochloric acid, so that the infusion system is obviously distinguished and obviously different from the known infusion system. This transfusion system constitutes with the conventional mercury atom fluorescence apparatus including reactor, atomizer, hollow cathode lamp and detector etc. the utility model discloses use water as the mercury atom fluorescence apparatus of current-carrying.
According to above design, utilize the utility model discloses a mercury atom fluorescence apparatus introduces the test solution of certain acidity and the reagent of certain concentration (being called the feed liquor) respectively simultaneously earlier at the infusion process, uses the pure water to get into the reactor reaction as current-carrying propelling movement respectively (carrier band propelling movement) test solution and reagent again, utilizes the atomizer to make the reaction back vapour atomization, and mercury fluorescence signal (being called the survey) is acquireed to rethread laser source and detector, and then mercury's concentration in obtaining the test solution. The infusion process completely does not use hydrochloric acid as a current carrier, and the current carrier of a reagent is changed into pure water, so that the infusion system is obviously different from a known infusion system and exceeds the conventional imagination.
The acidity (HCl%) of the test solution in mercury determination is 5% -10%, and the reducing agent NaBH4(or KBH4) The concentration was 0.2%. The measurable mercury concentration is below 5ng/ml, even at Hg concentrations as low as below 0.5ng/ml, below 0.1ng/ml (e.g., 0.04 ng/ml).
The mercury atomic fluorescence analyzer using water as carrier shown in fig. 1B is used to analyze mercury, and the specific steps may be as follows:
step 1, preparing systems with different mercury concentrationsPreparing standard solution, preparing sample solution to be tested, preparing NaBH4Placing the solution, standard solution and sample solution (collectively referred to as test solution) into a test solution bottle, and placing NaBH into the test solution bottle4Putting the solution (reagent for short) into a reagent bottle; purified water (as carrier water) is put into a water bottle.
Step 2, making a standard curve: 1) connecting a sample inlet pipe to a test solution bottle interface filled with standard blank liquid (acid liquid with the Hg concentration of 0), connecting a reagent inlet pipe to a reagent bottle interface, and feeding liquid (4-5 seconds); 2) switching a sample inlet pipe and a reagent inlet pipe to be communicated with a water inlet pipe, sucking carrier water into the sample inlet pipe and the reagent inlet pipe, and carrying a carrier tape to push blank liquid and a reagent; 3) the reactor, the atomizer and the excitation light source work, and the detector records a blank fluorescence value (from switching to the completion of detection of the detector for 8-10 seconds); 4) replacing the test solution bottles filled with standard solutions with different concentrations in sequence from low to high, and repeating the steps 1) -3), and sequentially measuring and obtaining the fluorescence value corresponding to each concentration standard solution in the standard series; 5) and drawing a mercury fluorescence value-concentration standard curve.
Step 3, sample determination: and (3) replacing the test solution bottle filled with the sample solution, repeating the steps 1) -3) to measure and obtain the fluorescence value corresponding to the sample solution, and converting the fluorescence value-concentration standard curve to obtain the concentration value of mercury in the sample solution. To avoid the residue of the high concentration mercury standard solution in the tube, the sample tube is preferably cleaned with water (as compared to the prior art using acid as a carrier, cleaning is not necessary, and even if cleaning, the amount of cleaning water is much less), before the sample solution is replaced, so that the memory effect of mercury can be better eliminated.
The utility model discloses use water as the mercury atom fluorescence apparatus of current-carrying, the infusion system of simplification is shown with reference to figure 2, include: the device comprises a test solution bottle for containing test solution and a reagent bottle for containing reducing agent, wherein the test solution bottle and the reagent bottle are respectively communicated with a reactor through a liquid inlet capillary tube inserted into liquid in the bottles, namely one end of the liquid inlet capillary tube is connected into the reactor, and the other end is a free end and is inserted into the solution in the test solution bottle or the reagent bottle; the two water bottles are used for containing purified water, one water bottle (water cup 1) contains cleaning water for cleaning a capillary tube, and the other water bottle (water cup 2) contains carrier flow water as a carrier flow. A peristaltic pump can be used in the infusion process of mercury atom fluorescence analysis, after a sample solution and a reagent are respectively input into a sample storage ring (called as sampling) through two capillaries under the action of the peristaltic pump, the front sections (free ends) of the two capillaries close to the head ends are transferred into the cleaning purified water of a water cup 1 to clean the solution adhered to the outer wall (shown by dotted lines in figure 2), then the head ends (free ends) of the two capillaries are transferred into a water cup 2 (shown by dotted lines in figure 2, the free ends of the capillaries are transferred into the water cup 1 from a sample solution bottle or a reagent bottle, and then transferred into the water cup 2 from the water cup 1 to be called as 'replacement insertion'), and the sample solution and the reagent in the sample storage ring are carried by current-carrying. Similarly, the reactor, the atomizer and the excitation light source work, namely mercury atom vapor generated by chemical reaction in the reactor is input into the atomizer and is excited by radiation of the mercury hollow cathode lamp. The emitted fluorescence signal is detected by a detector to obtain the concentration of mercury in the test solution.
The time control in the mercury atom fluorescence analysis by using the simplified liquid conveying system and taking water as a current carrier is as follows: sample/delay/add/drop (capillary)/assay: 4-5/0/2-3/8-10 (seconds). That is, the time for sucking in the sample solution and the reagent (sampling) is 4-5 seconds, the time delay is usually zero seconds, the capillary tube is taken out of the sample solution and the reagent, and the time for transferring the sample solution and the reagent into the water cup 2 (changing and inserting) after placing the sample solution and the reagent in the water cup 1 for a moment is usually 2-3 seconds. The time for pushing the test solution and the reagent in the sample storage ring by the carrier water in the water cup 2 until the end of the measurement is 8-10 seconds, and the fluorescence signal of the mercury is measured in the time.
The specific operation of the detection example is as follows:
operation 1. preparing mercury standard series solution and NaBH according to the requirement4Solutions and related reagents, sample solutions need to be prepared in advance. Placing a test solution bottle containing test solution and NaBH in a sample tray4A reagent bottle for the solution and two cups of purified water.
And 2, switching on a power supply of the atomic fluorescence instrument, confirming conditions required by the test, and lighting and preheating the hollow cathode lamp for 5-10 minutes. And opening the valve of the Ar gas steel cylinder, adjusting the pressure of the Ar gas to be 0.3MPA, and opening an exhaust device of the atomizer.
Operation 3, standard curve preparation:
1) sampling: the ends (free ends) of two liquid inlet capillary tubes are respectively inserted into a standard blank liquid and a reagent bottle of a test solution bottleNaBH of4In the solution, clicking a blank button of the instrument, executing an infusion program by the infusion system, and stopping the work of the peristaltic pump after sampling for 4-5 seconds;
2) immediately taking the free ends of the two capillaries out of the test solution bottle and the reagent bottle, firstly putting the capillaries into the cleaning water of the water cup 1 to clean so as to remove the attached solution, then transferring the capillaries into the purified water of the water cup 2 to finish the replacement and insertion (the replacement and insertion time is 2-3 seconds), and restarting the peristaltic pump after the two capillaries are inserted into the water cup 2;
3) the carrier water in the water cup 2 respectively enters the two capillary tubes under the action of the peristaltic pump, the carrier test solution and the reagent enter the reactor, the atomizer and the excitation light source work, the detector measures the fluorescence signal of the standard blank liquid and records the blank fluorescence value (the time from the carrier to the end of measurement is 8-10 seconds);
4) after the blank fluorescent signal is stable, the standard solution is a test solution, and 1) -3) is repeated to sequentially measure the fluorescent signals of the standard series solutions according to the concentration from low to high and record the fluorescent value; the peak curves of the fluorescence signals (fluorescence value-time) can be generated synchronously;
5) the concentration of the standard solution was inputted, and the average value of the measurement of each concentration of the standard solution was taken to prepare a fluorescence value-concentration standard curve.
Run 4. measurement of samples: after a liquid inlet capillary tube inserted into a test solution bottle is cleaned by water (the residue of high-concentration mercury standard solution in the tube is avoided, but the cleaning is not necessary at the place), clicking a sample test button of an instrument, firstly measuring the blank of a sample to be stable, taking the sample solution as the test solution, then pressing 1) -3 of operation 3) to respectively measure the fluorescence signals of the sample solutions, obtaining the concentration of mercury in the sample solution from 5) fluorescence value-concentration standard curve of operation 3 according to the fluorescence value of the sample, and calculating the content of mercury in the sample after inputting relevant parameters.
The measurement of atomic fluorescent mercury single element using water as carrier is introduced above. In practical applications, the mercury element can be measured with other elements, for example, by using a dual-channel atomic fluorescence analysis apparatus of the combined water-borne flow infusion system shown in fig. 1A, the infusion system of the apparatus is the same as that shown in fig. 1B or fig. 2, and one of the two excitation light sources is a mercury excitation light source. When the multi-element mercury is measured, standard mixed solution with different concentrations of each element is prepared, two excitation light sources are used for excitation based on the processes of one-time transfusion, reaction and atomization, the detector respectively obtains fluorescence signals of different elements, standard curves of corresponding elements are respectively made, the concentration of each element in each sample test solution is measured according to the steps and the operation, and the content of each element to be measured in the sample is calculated.
The analysis effect of mercury using the apparatus of the present invention is further illustrated below with reference to specific detection examples, in which the concentration of reagent "%" is expressed as mass percent concentration.
Example 1: analysis of Hg in associated uranium ore
Testing a sample: associated uranium mineral
This example utilizes a mercury atomic fluorescence meter with water as the carrier shown in FIG. 1B (the fluid delivery system is shown in FIG. 2).
Preparation of a mercury standard curve: a mercury standard solution of 50ng/ml Hg is prepared. 0, 1, 2, 3, 4 and 5ml of the standard solution are respectively taken and put into a 50ml plastic quantitative bottle, 5ml of HCl with the concentration of 50 percent is respectively added, the standard solution is diluted to the scale with water, and the Hg concentration in the obtained series of standard solutions is 0, 1, 2, 3, 4 and 5 ng/ml. The fluorescence signals of the blank and standard series solutions are measured according to the operation process, and the peak value curve of Hg is shown in A amplitude of figure 3, and a signal spectrum similar to Gaussian distribution is obtained. A fluorescence signal-concentration standard curve was prepared based on the fluorescence signal of the standard solution (see B panel in FIG. 3).
Preparation and determination of test solutions:
weighing 0.1-0.2g of an ore sample, placing the ore sample in 50ml of tetrafluoro sample dissolving tubes, adding 5ml of aqua regia with the concentration of 50% respectively, boiling and decomposing the ore sample in water bath for 1 hour, transferring the ore sample to a 50ml centrifuge tube by using water, adding 5ml of 50% HCl, diluting the ore sample to a scale by using water, shaking uniformly, taking the sample solution as a test solution, and determining a fluorescence signal of the sample solution according to the operation process. The Hg concentration was obtained from the standard curve and converted to Hg content in the sample. The results of the measurement of Hg in the sample are shown in Table 1.
TABLE 1 measurement of Hg in ore
| G(g) | Intensity of fluorescence | Concentration (ng/ml) | Volume of test solution (ml) | Sample content (μ g/g) |
| 0.1161 | 5046 | 1.699 | 50 | 0.528 |
| 0.2357 | 7264 | 2.447 | 50 | 0.521 |
| 0.1846 | 5645 | 1.901 | 50 | 0.517 |
| 0.1940 | 6038 | 2.033 | 50 | 0.524 |
As can be seen from the data in the table, under the condition that the sample weighing amount (G) is greatly different and the HCl concentration is 5%, the Hg in the ore can be rapidly measured by using a mercury determinator carrying water, the measured Hg content in the sample is almost the same, and the comparison result is consistent with the comparison result of a plurality of laboratories.
In the determination operation, only pure water (18.2M omega) is consumed without hydrochloric acid as a carrier, the sampling time is reduced by about 50 percent compared with the conventional method, and NaBH is reduced by about 50 percent4The solution only needs to be used for participating in the reaction, and is saved by more than 75% compared with the conventional detection. The sample weighing in the table is random, and it can be seen that the concentration of mercury in the solution is high or low, and the measurement can still be completed and a consistent result can be obtained, thus, the memory effect is eliminated by using water as a carrier, and even after the high-concentration standard solution is measured, the solution of the sample with other concentration is not influenced because the infusion system is cleaned by the carrier water.
Example 2: simultaneous measurement of Hg/As in soil
Testing a sample: soil(s)
Because the content of As in soil is much higher than Hg, the existing atomic fluorescence instrument can not simultaneously measure Hg and As in the sample. In the embodiment, two elements of Hg and As in the same sample are simultaneously detected by using water As a carrier current (by using a double-channel atomic fluorescence analysis device shown in FIG. 1A).
And (3) preparing a standard curve: a mixed standard solution containing 500ng/ml As and 10ng/ml Hg was prepared in advance. Taking 0, 1, 2, 3, 4 and 5ml of the standard solution respectively, putting 5ml of 5% Vc-5% thiourea solution and 10ml of HCl with the concentration of 50% into 50ml plastic quantitative bottles, diluting the bottles to a scale with water, and obtaining series of standard solutions with the Hg concentration of 0, 0.2, 0.4, 0.6, 0.8 and 1.0ng/ml and the As concentration of 0, 10, 20, 30, 40 and 50 ng/ml.
The fluorescence signals of Hg and As in the blank and standard series solutions were measured simultaneously by selecting the double-channel method, and standard curves of 0.2-1.0ng/ml Hg and 10-50ng/ml As of the mixed standard solution were prepared, respectively. The A panel of FIG. 4 is the peak value curve of Hg/As, and the B panel of FIG. 4 is the standard curve of mixed standard solution Hg and As (the signal of the standard curve is calculated from the spectrum area, and the blank area has been subtracted).
Preparation and determination of test solutions: 0.1-0.2g of soil sample is placed in a 50ml tetrafluoro sample dissolving tube, 50% aqua regia is added into the tube to be boiled and decomposed for 1 hour in water bath, the water is transferred into a 50ml plastic quantitative bottle, 5ml of 5% Vc-5% thiourea solution and 10ml of HCl with the concentration of 50% are added into the tube, the tube is diluted to scale with water, the sample solution is taken As a test solution to simultaneously measure the fluorescence signals of Hg and As according to the operation process after shaking up, and the concentration of corresponding elements is obtained according to respective standard curves so As to calculate the content of the elements in the sample. The results are shown in Table 2.
TABLE 2 results of simultaneous measurement of soil Hg/As
The data show that the difficulty of simultaneously measuring Hg and As in soil is solved using a water-borne atomic fluorescence method and apparatus. Meanwhile, the Hg concentration in 6 samples (standard samples) has larger difference, and the results of the samples sequentially tested from top to bottom according to the table 2 are consistent with the recommended values, which shows that the serious memory effect of Hg determination is eliminated by using the mercury atom fluorescence analysis method and device using water as a current carrying material.
In the embodiment, two elements coexist in the test solution, the conveying system only needs to finish the conveying of the test solution once, the detection of the double-channel detection system is also finished once, water is used as a current-carrying agent in the determination operation without hydrochloric acid, and NaBH is used in each analysis4The solution only needs to be prepared into 100ml-250ml for participating in the reaction, and the time and the cost of the whole testing process are greatly reduced.
Example 3: analysis of Hg in Rice
Testing a sample: rice
Preparation of a mercury standard curve: a standard mercury solution of 5ng/ml Hg was prepared. 0, 1, 2, 3, 4 and 5ml of the standard solution are respectively taken and put into a 50ml plastic quantitative bottle, 5ml of HCl with the concentration of 50 percent is respectively added, the standard solution is diluted to the scale with water, and the Hg concentration in the obtained series of standard solutions is 0, 0.1, 0.2, 0.3, 0.4 and 0.5 ng/ml. The fluorescence signals of the blank and standard series solutions were measured according to the procedure, the variation of the signal intensity with concentration is shown in A of FIG. 5, the peak curve is shown in B of FIG. 5, and a fluorescence signal-concentration standard curve (see C of FIG. 5) was prepared based on the fluorescence signals of the standard solutions.
Preparation and determination of test solutions:
weighing 0.3-0.5g of rice sample, placing the rice sample in 50ml tetrafluoro sample dissolving tubes, adding 5ml of aqua regia with the concentration of 50% respectively, boiling and decomposing the rice sample in water bath for 1 hour, transferring the rice sample to a 20ml centrifuge tube by using water, diluting the rice sample to a scale by using the water, measuring the fluorescence signal of the sample solution (considering that the maximum Hg concentration of the standard solution is only 0.5ng/ml, the Hg residue in the tube can be removed by using the water as a carrier, and the sample injection capillary does not need to be cleaned before being inserted into the sample solution), and obtaining the Hg concentration from the standard curve and converting the Hg concentration into the Hg content in the. The results of the measurement of Hg in the rice samples are shown in table 3.
TABLE 3 measurement of Hg in rice (ng/g)
It can be seen from the data in the table that Hg content in the rice is extremely low, is difficult to obtain accurate result with general analytical method, nevertheless adopts the utility model discloses the instrument is surveyed 4 rice samples, and the secondary parallel determination result is almost the same and coincide with the recommended value. Obviously, the utility model discloses use water to provide a reliable analytical means for detecting Hg in the rice for the atomic fluorescence appearance of current-carrying.
Claims (10)
1. The utility model provides an use mercury atom fluorescence apparatus of water as current-carrying, includes infusion system, reactor, atomizer, mercury hollow cathode lamp and detector, its characterized in that, infusion system includes examination liquid bottle, reagent bottle and water-jug, has held the pure water in the water-jug, and the water-jug delivery port communicates with the inlet of examination liquid bottle and reagent bottle respectively through two inlet tubes, is equipped with change over switch on the inlet tube, and the liquid outlet of examination liquid bottle and reagent bottle communicates with the reactor respectively.
2. The mercury atomic fluorescence tester using water as carrier according to claim 1, wherein the sample bottle is communicated with the reactor through a sample inlet tube, the reagent bottle is communicated with the reactor through a reagent inlet tube, and the sample inlet tube and the reagent inlet tube are both liquid inlet capillary tubes.
3. The apparatus of claim 2, further comprising a peristaltic pump, wherein the liquid inlet capillary of the sample inlet tube and the liquid inlet capillary of the reagent inlet tube are disposed in the peristaltic pump, and the liquid is respectively delivered to the reactors through the peristaltic pump.
4. The water-borne mercury atomic fluorescence spectrometer of claim 3, further comprising a sample ring, wherein the sample tube and the reagent tube extend from the rear end of the peristaltic pump to form respective sample rings.
5. A mercury atom fluorescence measuring instrument taking water as current carrying according to any one of claims 2 to 4, characterized in that one end of the liquid inlet capillary of the sample inlet pipe and the reagent inlet pipe is connected into the reactor, the other end is a free end to be inserted into the solution of the test solution bottle or the reagent bottle, the water bottle is two water cups, one water cup is used for containing cleaning water, the other water cup is used for containing current carrying water, the free end of the liquid inlet capillary is a water inlet pipe of the water bottle, and the free end of the liquid inlet capillary can be exchanged between the two water cups.
6. A liquid delivery system in a mercury atomic fluorescence tester taking water as a current carrier, which is specially used in the mercury atomic fluorescence tester taking water as a current carrier in any one of claims 1 to 5, and comprises a test solution bottle for containing a test solution and a reagent bottle for containing a reducing agent, and is characterized in that: the device also comprises a water bottle, purified water is contained in the water bottle, the water outlet of the water bottle is respectively communicated with the liquid inlets of the test solution bottle and the reagent bottle through two water inlet pipes, a change-over switch is arranged on the water inlet pipes, and the liquid outlets of the test solution bottle and the reagent bottle are respectively communicated with the reactor.
7. The fluid delivery system of claim 6, wherein the fluid delivery system comprises: the test solution bottle is communicated with the reactor through a sample inlet pipe, the reagent bottle is communicated with the reactor through a reagent inlet pipe, and the sample inlet pipe and the reagent inlet pipe are liquid inlet capillary tubes.
8. The liquid delivery system of claim 7, wherein the liquid inlet capillary of the sample inlet tube and the liquid inlet capillary of the reagent inlet tube are respectively filled in a peristaltic pump, and the peristaltic pumps are used for respectively delivering liquid to the reactors.
9. The fluid delivery system of claim 8, further comprising a sample ring, wherein the sample tube and the reagent tube extend into the respective sample rings at a rear end of the peristaltic pump.
10. The system according to any one of claims 7 to 9, wherein the inlet capillary of the sample inlet tube and the reagent inlet tube is connected to the reactor at one end and is inserted into the solution of the test solution bottle or the reagent bottle at the other end, the water bottles are two water bottles, one water cup is used for containing the cleaning water, the other water cup is used for containing the carrier water, the free end of the inlet capillary is the inlet tube of the water bottle, and the free end of the inlet capillary can be exchanged between the two water cups.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2018217606239 | 2018-10-29 | ||
| CN201821760623 | 2018-10-29 |
Publications (1)
| Publication Number | Publication Date |
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| CN209821067U true CN209821067U (en) | 2019-12-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111103268A (en) * | 2018-10-29 | 2020-05-05 | 重庆民泰新农业科技发展集团有限公司 | Mercury atom fluorescence tester using water as current carrying and mercury atom fluorescence analysis method |
| CN111103266A (en) * | 2018-10-29 | 2020-05-05 | 重庆民泰新农业科技发展集团有限公司 | Atomic fluorescence analysis method and analysis device using water as carrier |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111103268A (en) * | 2018-10-29 | 2020-05-05 | 重庆民泰新农业科技发展集团有限公司 | Mercury atom fluorescence tester using water as current carrying and mercury atom fluorescence analysis method |
| CN111103266A (en) * | 2018-10-29 | 2020-05-05 | 重庆民泰新农业科技发展集团有限公司 | Atomic fluorescence analysis method and analysis device using water as carrier |
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