CN217614776U - Hydride generating device of solid calcium hydride reducing agent - Google Patents
Hydride generating device of solid calcium hydride reducing agent Download PDFInfo
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- CN217614776U CN217614776U CN202221168197.6U CN202221168197U CN217614776U CN 217614776 U CN217614776 U CN 217614776U CN 202221168197 U CN202221168197 U CN 202221168197U CN 217614776 U CN217614776 U CN 217614776U
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The utility model discloses a hydride generating device of a solid calcium hydride reducing agent. The hydride generating device comprises a reaction bottle (1) with an open end and a cover body (2) matched with the open end of the reaction bottle (1); wherein, the cover body (2) is hermetically connected with a carrier gas inlet pipe (3), a hydride gas outlet pipe (4) and a sample inlet pipe (5) which extend into the reaction bottle (1); the carrier gas inlet pipe (3) is connected with a gas flowmeter (6); the cover body (2) is hermetically connected with the reaction bottle (1). The utility model adopts solid calcium hydride (10) as a reducing agent, avoids the use of a complex peristaltic pump or injection pump liquid-driving device, avoids the interference brought by a background value when carrying out atomic fluorescence detection, and has high detection sensitivity; acid is not needed in the whole analysis process, so that the detection cost is reduced, the analysis process is more environment-friendly, and the requirement of on-site measurement can be met.
Description
Technical Field
The utility model relates to an atomic fluorescence analysis field, concretely relates to hydride generating device of solid calcium hydride reductant.
Background
The atomic fluorescence photometer has the advantages of high sensitivity, low detection limit, support of multi-element analysis, wide linear range, no matrix interference and the like, and is widely used for measuring elements such as arsenic, mercury, selenium and the like. The fluorescence intensity is correlated with the concentration of mercury, and the concentration of the element to be measured is obtained by measuring the fluorescence signal of the mercury by a detector (usually a photomultiplier).
The current atomic fluorescence photometer mainly comprises: a sample introduction system, a gas-liquid separator, a carrier gas (usually argon), an atomizer, a high-performance hollow cathode lamp and a detector. The element aqueous solution to be detected, the acid and the reducing agent (borohydride solution) are pumped by a sample injection system and are mixed and reacted to generate the element gaseous hydride (or atomic vapor) to be detected, gas-liquid separation is realized in a gas-liquid separator, and the element gaseous hydride (or atomic vapor) to be detected enters an atomizer through the carrying of carrier gas (usually argon) and is excited to generate fluorescence for detection.
At present, potassium borohydride or sodium borohydride is adopted as a reducing agent to react with acid and an element to be detected on a mature atomic fluorescence photometer, a complex peristaltic pump or injection pump liquid driving device is adopted in the method, a sample flows in a pipeline to generate a memory effect, a background value is brought to measurement, interference is generated, and the sensitivity of the method is reduced; meanwhile, the method requires the use of a large amount of hydrochloric acid or nitric acid in the determination process, and obviously, the method can not meet the modern environment-friendly requirement more and more; in addition, the complicated liquid driving device of the peristaltic pump or the injection pump is difficult to realize the miniaturization of the instrument and can not meet the requirement of field measurement.
The applicant has found that the prior art has at least the following technical problems:
1. in the prior art, when an atomic fluorescence spectrophotometer is used for measurement, potassium borohydride or sodium borohydride is used as a reducing agent to react with acid and an element to be measured, and a complex peristaltic pump or injection pump liquid driving device is adopted, so that a sample flows in a pipeline, a memory effect is generated, a background value is brought to measurement, interference is generated, and the sensitivity of the method is reduced;
2. in the prior art, a large amount of hydrochloric acid or nitric acid is used in the measurement process by using an atomic fluorescence spectrophotometer, and if the generated wastewater is directly discharged to the environment, the wastewater treatment cost is increased if the wastewater is discharged after treatment;
3. when the atomic fluorescence photometer is used for detection in the prior art, the peristaltic pump or the injection pump liquid driving device is difficult to realize the miniaturization of an instrument and can not meet the requirement of on-site measurement.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a hydride generating device for atomic fluorescence photometer solid calcium hydride reductant to when solving among the prior art and using atomic fluorescence photometer to survey, all adopt potassium borohydride or sodium borohydride as reductant and acid and the element reaction that awaits measuring, owing to adopt complicated peristaltic pump or syringe pump to drive the liquid device, the sample flows in the pipeline, can produce memory effect, brings the background value to the survey, produces the interference, has reduced the technical problem of method sensitivity.
In order to achieve the above purpose, the utility model provides a following technical scheme:
the utility model provides a hydride generating device of solid calcium hydride reducing agent, which comprises a reaction bottle with an open end and a cover body matched with the open end of the reaction bottle; wherein the content of the first and second substances,
the cover body is hermetically connected with a carrier gas inlet pipe, a hydride gas outlet pipe and a sample inlet pipe which extend into the reaction bottle;
the carrier gas inlet pipe is connected with a gas flowmeter;
the cover body is connected with the reaction bottle in a sealing way.
Further, the gas inlet end of the carrier gas inlet pipe is connected with an external argon source, and the distance between the carrier gas inlet pipe and the inner surface of the bottom of the reaction bottle is 3-5cm; the distance between the hydride gas outlet pipe and the inner surface of the bottom of the reaction bottle is 7-9cm; the distance between the sample inlet pipe and the inner surface of the bottom of the reaction bottle is 3-5cm.
Further, the gas flowmeter is a gas mass flowmeter or a float flowmeter.
Furthermore, the sample inlet pipe is a sample inlet needle, and the cover body is provided with a sample inlet rubber mat at the position corresponding to the insertion position of the sample inlet needle and the positions where the carrier gas inlet pipe and the hydride gas outlet pipe are arranged; the sample injection rubber mat is embedded on the cover body, a carrier gas inlet hole, a hydride gas outlet hole and a sample inlet hole are formed in the sample injection rubber mat, and the carrier gas inlet pipe, the hydride gas outlet pipe and the sample inlet pipe are respectively installed in the carrier gas inlet hole, the hydride gas outlet hole and the sample inlet hole.
Furthermore, the cover body is in threaded connection with the reaction bottle, and a sealing rubber gasket is arranged at the position where the cover body is in contact with the top of the reaction bottle.
The hydride generation device using the solid calcium hydride reducing agent is used for atomic fluorescence analysis, and specifically comprises the following steps:
s1, preparing a sample to be detected, wherein the sample to be detected is a directly sampled aqueous solution, or a directly sampled solid sample is subjected to wet digestion and acid removal, and then a sample solution with a constant volume of deionized water is added;
s2, preparing standard solutions of the elements to be detected with different concentrations;
s3, weighing multiple parts of solid calcium hydride, respectively placing the multiple parts of solid calcium hydride in different reaction bottles, and correspondingly preparing a reaction bottle for containing the solid calcium hydride for each sample to be detected and each standard solution;
s4, setting carrier gas flow through a gas flowmeter, and introducing carrier gas into the reaction bottle;
s5, feeding a standard solution, wherein a cover body of a reaction bottle is covered at the open end of the reaction bottle during feeding, the standard solution with different concentrations sequentially enters the reaction bottle from a sample feeding pipe, and the standard solution reacts with solid calcium hydride to generate a gaseous substance of an element to be detected, hydrogen and waste liquid; the carrier gas loads the gaseous substance and the hydrogen of the element to be detected into the atomizer; burning hydrogen above the atomizer to form an argon-hydrogen flame; generating a ground state atom of the element to be detected in the argon-hydrogen flame by the gaseous substance of the element to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; the fluorescence signal is received by a detector, so that the content of the element to be detected in the standard solution with different concentrations is detected, and a standard curve equation can be calculated;
s6, sample introduction of a sample to be detected, wherein a cover body of a reaction bottle is covered at an open end of the reaction bottle during sample introduction, the sample to be detected enters the reaction bottle from a sample introduction pipe, and the sample to be detected reacts with solid calcium hydride to generate a gaseous substance of an element to be detected, hydrogen and waste liquid; the carrier gas loads the gaseous substance and the hydrogen of the element to be detected into the atomizer; burning hydrogen above the atomizer to form an argon-hydrogen flame; generating the ground state atoms of the elements to be detected in the argon-hydrogen flame by the gaseous substances of the elements to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; and (5) receiving the fluorescence signal by a detector, and finally obtaining the content of the element to be detected in the sample to be detected through the standard curve equation obtained in the step S5.
Further, in the step S3, the solid calcium hydride is in a powder form, and the weight amount of each solid calcium hydride is 0.2 to 2g.
Further, in the step S4, the carrier gas flow is set to be 100 to 1000mL/min.
Further, in the steps S5 and S6, the sample injection volumes of the standard solution and the sample to be detected are both 0.1-2mL.
Further, in the step S1, a sensitizer is added during the preparation of the sample solution, and the sensitizer is a mixed solution of sulfanilamide and ascorbic acid.
Based on the technical scheme, the embodiment of the utility model provides a can produce following technological effect at least:
(1) The utility model provides a hydride generating device of solid calcium hydride reductant adopts solid calcium hydride to be the reductant, has avoided the use that complicated peristaltic pump or syringe pump drove liquid device when carrying out atomic fluorescence detection, and then has avoided the interference that the background value brought, and detectivity is high.
(2) The utility model provides a hydride generating device of solid calcium hydride reducing agent is direct and the element aqueous solution that awaits measuring reacts and generates gaseous state material owing to adopt solid calcium hydride to be the reducing agent to need not to use acid in whole analytic process, when saving the cost, make analytic process more friendly to the environment.
(3) The utility model provides a hydride generating device of solid calcium hydride reductant adopts solid calcium hydride to be the reductant, and direct and the element aqueous solution that awaits measuring react and generate gaseous state material, and the gaseous state material that the carrier gas directly will generate loads into the atomizer, and the reaction bottle volume of adoption is small and exquisite, has avoided the use of complicated peristaltic pump or syringe pump flooding liquid device, can satisfy the requirement of site determination.
Drawings
FIG. 1 is a schematic structural diagram of embodiment 1 of the present invention;
FIG. 2 is a schematic view showing a structure of a reaction flask in example 1 of the present invention when solid calcium hydride is charged therein;
fig. 3 is a schematic structural view of a cover body in embodiment 1 of the present invention;
fig. 4 is a schematic connection diagram of the use state of embodiment 1 of the present invention;
fig. 5 is a diagram showing detection of Hg in application example 1 of the present invention;
FIG. 6 is a graph showing the detection of As in example 2 of the present invention;
in the figure: 1. a reaction bottle; 2. a cover body; 3. a carrier gas inlet pipe; 4. a hydride gas outlet pipe; 5. a sample inlet tube; 6. a gas flow meter; 7. an atomizer; 8. sampling a rubber mat; 9. sealing the rubber gasket; 10. solid calcium hydride; 11. a carrier gas inlet port; 12. hydride gas outlet holes; 13. and a sample inlet hole.
Detailed Description
As shown in fig. 1-6:
example 1:
the utility model provides a hydride generating device of solid calcium hydride reducing agent, which comprises a reaction bottle 1 with an open end and a cover body 2 matched with the open end of the reaction bottle 1; wherein the content of the first and second substances,
the cover body 2 is hermetically connected with a carrier gas inlet pipe 3, a hydride gas outlet pipe 4 and a sample inlet pipe 5 which extend into the reaction bottle 1;
the carrier gas inlet pipe 3 is connected with a gas flowmeter 6;
the cover body 2 is connected with the reaction bottle 1 in a sealing way.
The utility model provides a hydride generating device of solid calcium hydride reducing agent, which adopts solid calcium hydride 10 as the reducing agent, avoids the use of a complex peristaltic pump or injection pump liquid driving device, further avoids the interference caused by the background value, and has high detection sensitivity; because the solid calcium hydride 10 is used as a reducing agent and directly reacts with the element aqueous solution to be detected to generate gaseous substances, acid is not needed in the whole analysis process, the cost is saved, and the analysis process is more environment-friendly; in addition, as the solid calcium hydride 10 is used as a reducing agent and directly reacts with the element aqueous solution to be detected to generate the gaseous substance, the carrier gas directly loads the generated gaseous substance into the atomizer 7, the volume of the adopted reaction bottle 1 is small, the use of a complicated peristaltic pump or injection pump liquid driving device is avoided, and the requirement of on-site measurement can be met.
As an optional embodiment, the gas inlet end of the carrier gas inlet pipe 3 is connected with an external argon source, and the distance between the carrier gas inlet pipe 3 and the inner surface of the bottom of the reaction bottle 1 is 3-5cm; the distance between the hydride gas outlet pipe 4 and the inner surface of the bottom of the reaction bottle 1 is 7-9cm; the distance between the sample inlet pipe 5 and the inner surface of the bottom of the reaction bottle 1 is 3-5cm.
As an alternative embodiment, the gas flow meter 6 is a gas mass flow meter or a float flow meter.
As an optional implementation manner, the sample inlet tube 5 is a sample inlet needle, and the cover body 2 is provided with a sample inlet rubber mat 8 at a position corresponding to the insertion position of the sample inlet needle and the installation positions of the carrier gas inlet tube 3 and the hydride gas outlet tube 4; the sample injection rubber mat 8 is embedded on the cover body 2, a carrier gas inlet hole 11, a hydride gas outlet hole 12 and a sample inlet hole 13 are arranged on the sample injection rubber mat 8, and the carrier gas inlet pipe 3, the hydride gas outlet pipe 4 and the sample inlet pipe 5 are respectively arranged in the carrier gas inlet hole 11, the hydride gas outlet hole 12 and the sample inlet hole 13.
As an optional embodiment, the cover body 2 is in threaded connection with the reaction flask 1, and a sealing rubber gasket 9 is arranged at a position where the cover body 2 contacts with the top of the reaction flask 1.
Application example 1:
when the hydride generating device of the solid calcium hydride reducing agent in the embodiment 1 is used for atomic fluorescence analysis, the gas outlet of the hydride gas outlet pipe 4 is connected with the gas inlet end of the atomizer 7 on the atomic fluorescence photometer.
The method for measuring the Hg content in 4 national soil standard substances GBW07402, GBW07404, GBW07408 and GBW07428 specifically comprises the following steps:
s1, preparation of sample to be detected
Weighing 0.2500g of soil sample accurate to 0.0001g in a plastic tube with a plug, adding 5ml of a mixture of concentrated hydrochloric acid and concentrated nitric acid, shaking uniformly, boiling for 2h in a boiling water bath, and shaking once every 3-5min for multiple times in the process of the boiling water bath; cooling after boiling water bath, directly adding 2.5mL of mixed solution of sensitizer sulfanilamide and ascorbic acid after cooling, diluting to 25mL with water, and uniformly mixing to obtain sample solution;
the preparation method of the mixture of concentrated hydrochloric acid and concentrated nitric acid comprises the following steps: uniformly mixing commercially available concentrated hydrochloric acid with the concentration of 36-38% and commercially available concentrated nitric acid with the concentration of 68% according to the volume ratio of 1:1 to obtain a mixture of the concentrated hydrochloric acid and the concentrated nitric acid;
the preparation method of the mixed solution of sulfanilamide and ascorbic acid comprises the following steps: dissolving 5g of sulfanilamide in 100mL of aqueous solution to obtain sulfanilamide solution, and dissolving 5g of ascorbic acid in 100mL of aqueous solution to obtain ascorbic acid solution; uniformly mixing the sulfanilamide solution and the ascorbic acid solution to obtain a mixed solution of sulfanilamide and ascorbic acid;
s2, preparing standard solutions of elements to be detected with different concentrations
Preparing standard solutions with mercury contents of 0.00ng/ml, 1.00ng/ml, 2.00ng/ml, 4.00ng/ml, 6.00ng/ml and 8.00ng/ml respectively;
s3, weighing 10 parts of powdery solid calcium hydride 10, respectively placing the powdery solid calcium hydride 10 in different reaction bottles 1, wherein the weight of each part of the solid calcium hydride 10 is 0.2g, one reaction bottle 1 is correspondingly used for each standard solution with concentration, and one reaction bottle 1 is correspondingly used for each sample to be detected;
s4, setting the flow rate of carrier gas to be 600mL/min through the gas flowmeter 6, and introducing the carrier gas into the reaction bottle 1;
s5, feeding a standard solution, namely covering a cover body 2 of a reaction bottle 1 at the open end of the reaction bottle 1 during feeding, taking down the cover body 2 to cover the next reaction bottle 1 after the standard solutions with different concentrations enter the reaction bottle 1 from a sample feeding pipe 5 in sequence and feeding the standard solutions with different concentrations, wherein the feeding volume of each standard solution is 1mL, and the standard solutions react with solid calcium hydride 10 to generate gaseous substances, hydrogen and waste liquid of elements to be detected; the carrier gas loads the gaseous substance and the hydrogen of the element to be detected into the atomizer 7 through the hydride gas outlet pipe 4, and the working conditions of the atomizer 7 are set as follows: the current of the main cathode lamp is 20mA, the negative high voltage is 260V, the height of the atomization furnace is 10mm, the atomization temperature is 200 ℃, and the shielding gas flow is 300mL/min; the hydrogen gas is combusted above the atomizer 7 to form an argon-hydrogen flame; generating the ground state atoms of the elements to be detected in the argon-hydrogen flame by the gaseous substances of the elements to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; the fluorescence signals are received by a detector, so that the fluorescence values of standard series solutions containing 0.00ng/ml, 1.00ng/ml, 2.00ng/ml, 4.00ng/ml, 6.00ng/ml and 8.00ng/ml of mercury are respectively 20, 405, 631, 1169, 1662 and 2242; from this, a standard curve equation can be calculated, see fig. 5;
s6, sample introduction of a sample to be detected, wherein a cover body 2 of a reaction bottle 1 is covered at the open end of the reaction bottle 1 during sample introduction, the sample to be detected enters one sample to be detected in the reaction bottle 1 from a sample introduction pipe 5, the cover body 2 is taken down to cover the next reaction bottle 1, the cover body 2 is reused, the sample introduction volume of each sample to be detected is 1mL, and the sample to be detected reacts with solid calcium hydride 10 to generate a gaseous substance, hydrogen and waste liquid of an element to be detected; the carrier gas loads the gaseous substance of the element to be detected and the hydrogen into the atomizer 7 to set the working conditions of the atomizer 7: the current of a main cathode lamp is 20mA, the negative high voltage is 260V, the height of the atomization furnace is 10mm, the atomization temperature is 200 ℃, and the shielding gas flow is 300mL/min; the hydrogen gas is combusted above the atomizer 7 to form an argon-hydrogen flame; generating the ground state atoms of the elements to be detected in the argon-hydrogen flame by the gaseous substances of the elements to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; and receiving the fluorescence signal by a detector, and obtaining the content of Hg in the sample to be detected through a standard curve equation.
The results of the measurement of Hg content are shown in table 1 below:
TABLE 1Hg content measurement results
| Soil sample numbering | Hg standard value [ mu ] g/g | Hg measurement μ g/g |
| GBW07402 | 0.015±0.003 | 0.0172 |
| GBW07404 | 0.59±0.05 | 0.548 |
| GBW07408 | 0.017±0.003 | 0.0150 |
| GBW07428 | 0.089±0.004 | 0.0862 |
Application example 2:
when the hydride generator of the solid calcium hydride reducing agent in the embodiment 1 is used for atomic fluorescence analysis, the gas outlet of the hydride gas outlet pipe 4 is connected with the gas inlet end of the atomizer 7 on the atomic fluorescence photometer.
The method for measuring the As content in 4 national soil standard substances GBW07402, GBW07404, GBW07408 and GBW07428 specifically comprises the following steps:
s1, preparation of sample to be detected
Weighing 0.1000g of soil sample accurate to 0.0001g in a plastic tube with a plug, adding 5ml of a mixture of concentrated hydrochloric acid and concentrated nitric acid, shaking uniformly, boiling for 2h in a boiling water bath, and shaking once every 3-5min for multiple times in the process of the boiling water bath; cooling after boiling water bath, directly adding 2.5mL of mixed solution of sensitizer sulfanilamide and ascorbic acid after cooling, diluting to 25mL with water, and uniformly mixing to obtain sample solution;
the preparation method of the mixture of concentrated hydrochloric acid and concentrated nitric acid comprises the following steps: uniformly mixing commercially available concentrated hydrochloric acid with the concentration of 36-38% and commercially available concentrated nitric acid with the concentration of 68% according to the volume ratio of 1:1 to obtain a mixture of the concentrated hydrochloric acid and the concentrated nitric acid;
the preparation method of the mixed solution of sulfanilamide and ascorbic acid comprises the following steps: dissolving 5g of sulfanilamide in 100mL of aqueous solution to obtain sulfanilamide solution, and dissolving 5g of ascorbic acid in 100mL of aqueous solution to obtain ascorbic acid solution; uniformly mixing the sulfanilamide solution and the ascorbic acid solution to obtain a mixed solution of sulfanilamide and ascorbic acid;
s2, preparing standard solutions of elements to be detected with different concentrations
Preparing standard solutions with As respectively being 0.00ng/ml, 10.00ng/ml, 20.00ng/ml, 30.00ng/ml, 40.00ng/ml and 60.00 ng/ml;
s3, weighing 10 parts of powdery solid calcium hydride 10, respectively placing the powdery solid calcium hydride 10 in different reaction bottles 1, wherein the weight of each part of solid calcium hydride 10 is 2g, one reaction bottle 1 is correspondingly used for each standard solution with each concentration, and one reaction bottle 1 is correspondingly used for each sample to be detected;
s4, setting the flow of carrier gas to be 1000mL/min through a gas flowmeter 6, and introducing carrier gas into the reaction bottle 1;
s5, sample introduction of standard solutions, namely covering a cover body 2 of a reaction bottle 1 at the open end of the reaction bottle 1 during sample introduction, allowing the standard solutions with different concentrations to enter the reaction bottle 1 from a sample introduction pipe 5 in sequence, taking down the cover body 2 to cover the next reaction bottle 1 after sample introduction of the standard solutions with one concentration is finished, reusing the cover body 2, wherein the sample introduction volume of each standard solution is 2mL, and reacting the standard solutions with solid calcium hydride 10 to generate gaseous substances, hydrogen and waste liquid of elements to be detected; the carrier gas loads the gaseous substance of the element to be detected and the hydrogen into the atomizer 7 through the hydride gas outlet pipe 4, and the working conditions of the atomizer 7 are set as follows: the current of the main cathode lamp is 20mA, the negative high voltage is 260V, the height of the atomization furnace is 10mm, the atomization temperature is 200 ℃, and the shielding gas flow is 300mL/min; the hydrogen gas is combusted above the atomizer 7 to form an argon-hydrogen flame; generating the ground state atoms of the elements to be detected in the argon-hydrogen flame by the gaseous substances of the elements to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; the fluorescence signals are received by a detector, so that the fluorescence values of standard series solutions containing As respectively 0.00ng/ml, 10.00ng/ml, 20.00ng/ml, 30.00ng/ml, 40.00ng/ml and 60.00ng/ml are respectively 15, 419, 794, 1274 and 1584,2571; from this, a standard curve equation (see fig. 6) can be calculated;
s6, sample introduction of a sample to be detected, wherein a cover body 2 of a reaction bottle 1 is covered at the open end of the reaction bottle 1 during sample introduction, the sample to be detected enters one sample to be detected in the reaction bottle 1 from a sample introduction pipe 5, the cover body 2 is taken down to cover the next reaction bottle 1, the cover body 2 is reused, the sample introduction volume of each sample to be detected is 2mL, and the sample to be detected reacts with solid calcium hydride 10 to generate a gaseous substance, hydrogen and waste liquid of an element to be detected; the carrier gas loads the gaseous substance of the element to be detected and the hydrogen into the atomizer 7 to set the working conditions of the atomizer 7: the current of the main cathode lamp is 20mA, the negative high voltage is 260V, the height of the atomization furnace is 10mm, the atomization temperature is 200 ℃, and the shielding gas flow is 300mL/min; the hydrogen gas is combusted above the atomizer 7 to form an argon-hydrogen flame; generating the ground state atoms of the elements to be detected in the argon-hydrogen flame by the gaseous substances of the elements to be detected; the ground state atoms generate fluorescent signals under the irradiation of a light source; the fluorescence signal is received by the detector, and the content of As in the sample to be detected is obtained through a standard curve equation.
The results of the As content measurement are shown in Table 2 below:
TABLE 2 determination of As content
| Soil sample number | As standard value μ g/g | As measurement value μ g/g |
| GBW07402 | 13.7±1.2 | 12.79 |
| GBW07404 | 58±6 | 52.8 |
| GBW07408 | 12.7±1.1 | 13.32 |
| GBW07428 | 6.5±1.3 | 7.65 |
While the present invention has been described with reference to the exemplary embodiments of the present invention in which solid calcium hydride is used as the reducing agent, it is to be understood that the terminology used is intended to be in the nature of words of description and illustration, rather than of limitation. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the metes and bounds of the claims, or equivalence of such metes and bounds are therefore intended to be embraced by the appended claims.
Claims (5)
1. A hydride generating device of solid calcium hydride reducing agent is characterized by comprising a reaction bottle (1) with an open end and a cover body (2) matched with the open end of the reaction bottle (1); wherein the content of the first and second substances,
the cover body (2) is hermetically connected with a carrier gas inlet pipe (3), a hydride gas outlet pipe (4) and a sample inlet pipe (5) which extend into the reaction bottle (1);
the carrier gas inlet pipe (3) is connected with a gas flowmeter (6);
the cover body (2) is hermetically connected with the reaction bottle (1).
2. The hydride generator of solid calcium hydride reducing agent as claimed in claim 1, wherein the inlet end of the carrier gas inlet tube (3) is connected to an external argon source, and the distance between the carrier gas inlet tube (3) and the inner surface of the bottom of the reaction flask (1) is 3-5cm; the distance between the hydride gas outlet pipe (4) and the inner surface of the bottom of the reaction bottle (1) is 7-9cm; the distance between the sample inlet pipe (5) and the inner surface of the bottom of the reaction bottle (1) is 3-5cm.
3. The hydride generator of a solid calcium hydride reducing agent according to claim 1, wherein the gas flow meter (6) is a gas mass flow meter or a float flow meter.
4. The hydride generating device of the solid calcium hydride reducing agent according to claim 1, wherein the sample inlet tube (5) is a sample injection needle, and the cover body (2) is provided with a sample injection rubber cushion (8) at a position corresponding to the insertion of the sample injection needle and the positions where the carrier gas inlet tube (3) and the hydride gas outlet tube (4) are installed; advance kind cushion (8) and inlay and establish on lid (2), be equipped with carrier gas inlet port (11), hydride gas venthole (12) and sample inlet hole (13) on advance kind cushion (8), install respectively in carrier gas inlet port (11), hydride gas venthole (12) and sample inlet hole (13) carrier gas inlet pipe (3), hydride gas outlet duct (4) and sample inlet pipe (5).
5. The hydride generator of solid calcium hydride reducer as claimed in claim 1, wherein the cover (2) is screwed to the reaction flask (1), and a sealing rubber gasket (9) is provided at a position where the cover (2) contacts with the top of the reaction flask (1).
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| CN202221168197.6U CN217614776U (en) | 2022-05-16 | 2022-05-16 | Hydride generating device of solid calcium hydride reducing agent |
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