阅读说明：本技术 一种使用原子荧光测定土壤及沉积物砷的检测方法 (Detection method for measuring arsenic in soil and sediment by using atomic fluorescence ) 是由 周艳春 于 2019-11-08 设计创作，主要内容包括：本发明公开了一种使用原子荧光测定土壤及沉积物砷的检测方法,包括步骤一,土壤勘测；步骤二,土壤取样；步骤三,测定试剂制作；步骤四,原子荧光测定；步骤五,测定结果观测；步骤六,档案归纳存储；步骤七,后期数据对比；其中在上述步骤一中,人工选择污染严重的土壤,使用围栏围起选择的土壤,保证土壤的完整性；该一种使用原子荧光测定土壤及沉积物砷的检测方法,采用王水浸提法,不会破坏测试的土壤,同时可以使土壤中的沉积物砷元素原子化,使其基态原子被激发至高能态,发射特征波长的原子荧光,再利用原子荧光测定仪器即可测定土壤及沉积物砷,针对性强,克服了土壤其他金属元素的干扰,提升了准确度与精确度。(The invention discloses a detection method for measuring arsenic in soil and sediment by using atomic fluorescence, which comprises the following steps of firstly, surveying the soil; step two, sampling soil; step three, preparing a determination reagent; step four, atomic fluorescence measurement; step five, observing a measuring result; step six, the files are summarized and stored; step seven, comparing the later data; in the first step, soil with serious pollution is manually selected, and the selected soil is enclosed by a fence to ensure the integrity of the soil; according to the detection method for measuring the arsenic in the soil and the sediment by using the atomic fluorescence, the tested soil is not damaged by adopting the aqua regia leaching method, meanwhile, the arsenic in the sediment in the soil can be atomized, the ground state atoms of the arsenic are excited to a high energy state, the atomic fluorescence with characteristic wavelength is emitted, the arsenic in the soil and the sediment can be measured by using an atomic fluorescence measuring instrument, the pertinence is high, the interference of other metal elements in the soil is overcome, and the accuracy and precision are improved.)

1. A detection method for measuring arsenic in soil and sediment by using atomic fluorescence comprises the steps of firstly, surveying the soil; step two, sampling soil; step three, preparing a determination reagent; step four, atomic fluorescence measurement; step five, observing a measuring result; step six, the files are summarized and stored; step seven, comparing the later data; the method is characterized in that:

wherein in step one above, the soil survey comprises the steps of:

1) manually selecting seriously polluted soil, and enclosing the selected soil by using a fence to ensure the integrity of the soil;

2) observing the soil for ten days, manually recording the vegetation growth condition around the soil, and determining the soil pollution severity;

wherein in the second step, the soil sampling comprises the following steps:

1) manually pouring a small amount of water into the selected soil for wetting, and manually turning and finishing;

2) selecting soil with complete samples, wrapping the soil, and then storing the soil in a shady and cool place;

in the third step, the preparation of the measuring reagent comprises the following steps:

1) manually mixing 3 parts of concentrated hydrochloric acid and 1 part of concentrated nitric acid, diluting by 1 time with pure water to prepare aqua regia solution, and storing in shade;

2) mixing 5% of thiourea and 5% of ascorbic acid under stirring, dissolving the mixture in water to obtain a reducing agent, and storing in shade;

wherein in the fourth step, the atomic fluorescence measurement comprises the following steps:

1) drying the soil selected in the step 2), manually crushing, and screening by using a 100-mesh screen;

2) placing the screened soil into a colorimetric tube or other test tubes, shaking the test tubes to loosen the soil and ensuring that the soil occupies one third of the volume of the test tubes;

3) pouring the aqua regia solution obtained in the step three 1), covering the top of the test tube with a breathable glass plug, soaking for 24h, shaking once every 1h, heating for 2h by using a water bath, taking out the test tube after heating, cooling to room temperature, and standing for 24 h;

4) taking supernatant of the test tube after standing, adding the reducing agent in the step three 2), manually shaking for 20min, adding concentrated hydrochloric acid, and standing for 30-50 min;

5) preheating an atomic fluorescence measuring instrument for 20min after setting working conditions, and placing the mixed liquid in the test tube into the instrument after the instrument is stable to measure;

in the fifth step, observing whether fluorescence exists manually through an instrument, and simultaneously automatically drawing atomic fluorescence with characteristic wavelength by a computer;

in the sixth step, the result of the manual observation and the result recorded by the computer are stored in a file room and a computer respectively for comparison again;

and seventhly, manually recording observation data at intervals, and simultaneously comparing the data.

2. The method for detecting arsenic in soil and sediments by atomic fluorescence as claimed in claim 1, wherein the method comprises the following steps: in the step one 2), the recorded data is stored in an archive room for subsequent comparison.

3. The method for detecting arsenic in soil and sediments by atomic fluorescence as claimed in claim 1, wherein the method comprises the following steps: in the second step 2), the stored soil is observed manually every 2 hours and recorded.

4. The method for detecting arsenic in soil and sediments by atomic fluorescence as claimed in claim 1, wherein the method comprises the following steps: in the third step, the aqua regia solution and the reducing agent can also be stored in a refrigerator at low temperature.

5. The method for detecting arsenic in soil and sediments by atomic fluorescence as claimed in claim 1, wherein the method comprises the following steps: in the step four 1), the soil can also be crushed by using a crusher.

6. The method for detecting arsenic in soil and sediments by atomic fluorescence as claimed in claim 1, wherein the method comprises the following steps: in the seventh step, the observation and recording are carried out once every 30 min.

Technical Field

The invention relates to the field of soil determination, in particular to a detection method for determining arsenic in soil and sediments by using atomic fluorescence.

Background

The soil is formed and evolved under the comprehensive action of various soil forming factors such as parent material, climate, biology, terrain, time and the like, the soil is very complex in composition and generally consists of solid, liquid and gas phases such as organic matters, moisture and air generated by decay of mineral matters and animal and plant residues, and due to the serious pollution at present, arsenic in soil sediments is increased, the growth of vegetation is not facilitated, and the environment pollution is caused; the traditional detection of the arsenic in the soil and the sediment adopts manual sampling, and the detection is carried out by using an instrument, so that the time and the labor are wasted, the detection is single, the accuracy is low, and the detection result is easily influenced by other metal objects in the soil, so that the detection is not beneficial to a user; in view of these drawbacks, it is necessary to design a detection method for measuring arsenic in soil and sediments by using atomic fluorescence.

Disclosure of Invention

The invention aims to provide a detection method for measuring arsenic in soil and sediment by using atomic fluorescence, which solves the problems in the background technology.

In order to solve the technical problems, the invention provides the following technical scheme: a detection method for measuring arsenic in soil and sediment by using atomic fluorescence comprises the steps of firstly, surveying the soil; step two, sampling soil; step three, preparing a determination reagent; step four, atomic fluorescence measurement; step five, observing a measuring result; step six, the files are summarized and stored; step seven, comparing the later data;

wherein in step one above, the soil survey comprises the steps of:

1) manually selecting seriously polluted soil, and enclosing the selected soil by using a fence to ensure the integrity of the soil;

2) observing the soil for ten days, manually recording the vegetation growth condition around the soil, and determining the soil pollution severity;

wherein in the second step, the soil sampling comprises the following steps:

1) manually pouring a small amount of water into the selected soil for wetting, and manually turning and finishing;

2) selecting soil with complete samples, wrapping the soil, and then storing the soil in a shady and cool place;

in the third step, the preparation of the measuring reagent comprises the following steps:

1) manually mixing 3 parts of concentrated hydrochloric acid and 1 part of concentrated nitric acid, diluting by 1 time with pure water to prepare aqua regia solution, and storing in shade;

2) mixing 5% of thiourea and 5% of ascorbic acid under stirring, dissolving the mixture in water to obtain a reducing agent, and storing in shade;

wherein in the fourth step, the atomic fluorescence measurement comprises the following steps:

1) drying the soil selected in the step 2), manually crushing, and screening by using a 100-mesh screen;

2) placing the screened soil into a colorimetric tube or other test tubes, shaking the test tubes to loosen the soil and ensuring that the soil occupies one third of the volume of the test tubes;

3) pouring the aqua regia solution obtained in the step three 1), covering the top of the test tube with a breathable glass plug, soaking for 24h, shaking once every 1h, heating for 2h by using a water bath, taking out the test tube after heating, cooling to room temperature, and standing for 24 h;

4) taking supernatant of the test tube after standing, adding the reducing agent in the step three 2), manually shaking for 20min, adding concentrated hydrochloric acid, and standing for 30-50 min;

5) preheating an atomic fluorescence measuring instrument for 20min after setting working conditions, and placing the mixed liquid in the test tube into the instrument after the instrument is stable to measure;

in the fifth step, observing whether fluorescence exists manually through an instrument, and simultaneously automatically drawing atomic fluorescence with characteristic wavelength by a computer;

in the sixth step, the result of the manual observation and the result recorded by the computer are stored in a file room and a computer respectively for comparison again;

and seventhly, manually recording observation data at intervals, and simultaneously comparing the data.

According to the technical scheme, in the step one 2), the recorded data is stored in an archive room for subsequent comparison.

According to the technical scheme, in the step two 2), the stored soil is observed manually every 2 hours and recorded.

According to the technical scheme, in the third step, the aqua regia solution and the reducing agent can also be stored in a refrigerator at low temperature.

According to the technical scheme, in the step four 1), the soil can also be crushed by using a crusher.

According to the technical scheme, in the seventh step, observation and recording are carried out once every 30 min.

Compared with the prior art, the invention has the following beneficial effects: the method for detecting the arsenic in the soil and the sediment by using the atomic fluorescence adopts the aqua regia leaching method, the tested soil cannot be damaged, meanwhile, the arsenic in the sediment in the soil can be atomized, the ground state atoms are excited to a high energy state and then return to the ground state from the high energy state, the atomic fluorescence with characteristic wavelength is emitted, the arsenic in the soil and the sediment can be detected by using an atomic fluorescence detecting instrument, the method is time-saving, labor-saving, convenient, fast and highly targeted, the interference of other metal elements in the soil is overcome, the accuracy and precision are greatly improved, and the detection by a user is facilitated.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:

FIG. 1 is a flow chart of the method of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1, the present invention provides a technical solution:

a detection method for measuring arsenic in soil and sediment by using atomic fluorescence comprises the steps of firstly, surveying the soil; step two, sampling soil; step three, preparing a determination reagent; step four, atomic fluorescence measurement; step five, observing a measuring result; step six, the files are summarized and stored; step seven, comparing the later data;

wherein in step one above, the soil survey comprises the steps of:

1) manually selecting seriously polluted soil, and enclosing the selected soil by using a fence to ensure the integrity of the soil;

2) observing the soil for ten days, manually recording the vegetation growth condition around the soil, determining the soil pollution severity, and storing the recorded data in a file room for subsequent comparison;

wherein in the second step, the soil sampling comprises the following steps:

1) manually pouring a small amount of water into the selected soil for wetting, and manually turning and finishing;

2) selecting complete soil of a sample, wrapping the soil, placing the wrapped soil in a shady and cool place for storage, manually observing the stored soil every 2 hours, and recording;

in the third step, the preparation of the measuring reagent comprises the following steps:

1) manually mixing 3 parts of concentrated hydrochloric acid and 1 part of concentrated nitric acid, diluting by 1 time with pure water to prepare aqua regia solution, and storing in shade;

2) mixing 5% of thiourea and 5% of ascorbic acid under stirring, dissolving the mixture in water to obtain a reducing agent, and storing in shade, or storing the aqua regia solution and the reducing agent in a refrigerator at low temperature;

wherein in the fourth step, the atomic fluorescence measurement comprises the following steps:

1) drying the soil selected in the step 2), manually crushing the soil, or crushing the soil by using a crusher, and screening the soil by using a 100-mesh screen;

2) placing the screened soil into a colorimetric tube or other test tubes, shaking the test tubes to loosen the soil and ensuring that the soil occupies one third of the volume of the test tubes;

3) pouring the aqua regia solution obtained in the step three 1), covering the top of the test tube with a breathable glass plug, soaking for 24h, shaking once every 1h, heating for 2h by using a water bath, taking out the test tube after heating, cooling to room temperature, and standing for 24 h;

4) taking supernatant of the test tube after standing, adding the reducing agent in the step three 2), manually shaking for 20min, adding concentrated hydrochloric acid, and standing for 30-50 min;

5) preheating an atomic fluorescence measuring instrument for 20min after setting working conditions, and placing the mixed liquid in the test tube into the instrument after the instrument is stable to measure;

in the fifth step, observing whether fluorescence exists manually through an instrument, and simultaneously automatically drawing atomic fluorescence with characteristic wavelength by a computer;

in the sixth step, the result of the manual observation and the result recorded by the computer are stored in a file room and a computer respectively for comparison again;

and in the seventh step, manually recording observation data at intervals, simultaneously comparing the data, and observing and recording once every 30 min.

Based on the above, the method has the advantages that the method adopts the aqua regia leaching method, the tested soil is not damaged, meanwhile, the arsenic in the sediment in the soil can be atomized, the ground state atoms are excited to a high energy state, then the high energy state returns to the ground state, the atomic fluorescence with characteristic wavelength is emitted, and the soil and the arsenic in the sediment can be measured by using an atomic fluorescence measuring instrument.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.