CN113702310A - Pyroelectric reagent for analyzing cadmium in soil and use method - Google Patents
Pyroelectric reagent for analyzing cadmium in soil and use method Download PDFInfo
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- CN113702310A CN113702310A CN202111083703.1A CN202111083703A CN113702310A CN 113702310 A CN113702310 A CN 113702310A CN 202111083703 A CN202111083703 A CN 202111083703A CN 113702310 A CN113702310 A CN 113702310A
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 92
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 74
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000002689 soil Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 43
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 170
- 239000001103 potassium chloride Substances 0.000 claims abstract description 69
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 69
- 239000007864 aqueous solution Substances 0.000 claims abstract description 30
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 87
- 235000006408 oxalic acid Nutrition 0.000 claims description 29
- 239000004115 Sodium Silicate Substances 0.000 claims description 28
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 28
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000012360 testing method Methods 0.000 claims description 18
- 239000006004 Quartz sand Substances 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 14
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 239000010453 quartz Substances 0.000 description 8
- 238000001149 thermolysis Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000000120 microwave digestion Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a heat release reagent for analyzing cadmium in soil, which comprises potassium chloride, wherein the potassium chloride is potassium chloride particles or saturated potassium chloride aqueous solution. The application also provides a use method of the thermolytic reagent for analyzing cadmium in soil. The heat release reagent provided by the application is introduced into an electrothermal evaporation-hydrogen flame atomization-atomic absorption method, so that the recovery rate of direct determination of cadmium in soil can be effectively improved, and the aim of accurately determining the content of cadmium in soil is fulfilled.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a thermolysis reagent for analyzing cadmium in soil and a using method thereof.
Background
At present, the method for accurately measuring cadmium in soil mainly uses corrosive reagents such as sulfuric acid, nitric acid, hydrochloric acid, hydrofluoric acid, hydrogen peroxide and the like, prepares a soil sample into a uniform solution state by means of pretreatment means such as a microwave digestion instrument, a hot plate digestion instrument, a high-pressure tank digestion instrument and the like, and then measures cadmium in the solution by using a graphite furnace atomic absorption photometer, an inductively coupled plasma emission spectrum, a chemical steam generation atomic fluorescence photometer, an inductively coupled plasma mass spectrometer and the like. The analysis process is complex, takes long time, easily brings many factors of analysis errors, has high analysis cost and causes environmental pollution in the analysis process.
Chinese patent publication No. CN110579564A discloses a method for detecting cadmium, which adopts an electrothermal evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method "to achieve accurate determination of mercury, cadmium, zinc and lead, so that the method is an effective method for achieving direct determination of cadmium in soil samples, and compared with the classical graphite furnace atomic absorption method requiring complex chemical pretreatment, inductively coupled plasma mass spectrometry and other methods, the method has high sensitivity and can directly and rapidly determine cadmium in soil samples without chemical pretreatment.
But the experiment proves that: the method for directly measuring cadmium in the soil sample by adopting an electric heating evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method is adopted, and when the soil sample with high calcium and high magnesium content is encountered, the measurement recovery rate of cadmium is usually low, but the low trend has no obvious correlation with the calcium and magnesium content. The complexity of the matrix of the soil sample and the occurrence form diversity of cadmium in the soil sample cause that the cadmium in the soil cannot be accurately and quantitatively analyzed when an electrothermal evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method is applied.
Disclosure of Invention
The invention aims to provide a thermolysis reagent for analyzing cadmium in soil, which can accurately determine the content of cadmium in soil.
In view of the above, the present application provides a thermolysis reagent for analyzing cadmium in soil, comprising potassium chloride, wherein the potassium chloride is potassium chloride particles or a saturated potassium chloride aqueous solution.
Preferably, when the potassium chloride is potassium chloride particles, the heat release reagent further comprises oxalic acid and quartz sand; the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.5): (0.01-0.3): 1.
preferably, the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.3): (0.01-0.1): 1.
preferably, when the potassium chloride is a saturated potassium chloride aqueous solution, the heat release reagent further comprises oxalic acid and sodium silicate, and the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.5): (0.001-0.03): 1.
preferably, the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.3): (0.001-0.01): 1.
preferably, when the potassium chloride is a saturated potassium chloride aqueous solution, the heat release reagent further comprises sodium silicate, and the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001-0.03).
Preferably, the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001-0.01).
Preferably, the content of cadmium in the soil is 0.01-100 mg/kg, and the mass ratio of the potassium chloride to the cadmium in the soil is (5-200): (0.00001 to 1).
The application also provides a using method of the heat release reagent, which comprises the following steps:
paving a pyroelectric reagent at the bottom of a loading part, placing a soil sample on the surface of the pyroelectric reagent, placing the loading part on a sample introduction part of a detection instrument, and starting testing; the pyroelectric reagent comprises potassium chloride particles;
or, dripping the heat releasing reagent on the soil sample of the loading part to enable the heat releasing reagent to fully infiltrate the soil sample, then placing the loading part on a sample introduction part of the detection instrument, and starting the test; the heat releasing reagent comprises a saturated potassium chloride aqueous solution;
or, the pyroelectric reagent is placed in a loading part, dried and sealed to obtain a modified pyroelectric reagent loading part which is used as a disposable modified loading part; the disposable modified loading component can directly weigh a soil sample to start testing; the pyroelectric reagent comprises a saturated aqueous solution of potassium chloride.
Preferably, the detection instrument is an AA2288 full-automatic cadmium detector; the analysis wavelength of the full-automatic cadmium detector is 228.8nm, the lamp current is 5.0mA, the negative high voltage of the PMT is-360V, and the atomizer is hydrogen flame; the detecting step comprises drying, temperature rising, pyrolysis and gas switching.
The application provides a heat release reagent for analyzing cadmium in soil, which comprises potassium chloride as a basic component, wherein the potassium chloride can be potassium chloride particles or saturated potassium chloride aqueous solution. The heat release reagent provided by the application is introduced into an electrothermal evaporation-hydrogen flame atomization-atomic absorption method, so that the recovery rate of direct determination of cadmium in soil can be effectively improved, and the aim of accurately determining the content of cadmium in soil is fulfilled.
Drawings
FIG. 1 is a peak diagram of a soil sample before and after the soil sample is added with a pyroelectric reagent;
FIG. 2 is a graph showing comparative analysis of results obtained before and after addition of different pyroelectric reagents and results obtained by a GF-AAS method.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the problem that the method provided by the prior art cannot accurately and quantitatively analyze cadmium in soil, the application introduces a heat release reagent in the method of electrothermal evaporation (heating a quartz tube) -hydrogen flame atomization-atomic absorption method, which can effectively improve the recovery rate of direct determination of cadmium in soil, thereby achieving the purpose of accurately determining the content of cadmium in soil. The embodiment of the invention discloses a heat release reagent for analyzing cadmium in soil, which comprises potassium chloride, wherein the potassium chloride is potassium chloride particles or saturated potassium chloride aqueous solution.
In this application, when potassium chloride is potassium chloride granule, heat releases reagent still includes oxalic acid and quartz sand, the mass ratio of oxalic acid, quartz sand and potassium chloride is (0.01 ~ 0.5): (0.01-0.3): 1; more specifically, the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.3): (0.01-0.25): 1; in a specific embodiment, the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.3): (0.01-0.2): 1.
when the potassium chloride is a saturated potassium chloride aqueous solution, the heat release reagent further comprises oxalic acid and sodium silicate, and the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.5): (0.001-0.03): 1; more specifically, the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.3): (0.001-0.01): 1; in a specific embodiment, the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.08-0.28): (0.002-0.008): 1. similarly, when the potassium chloride is a saturated potassium chloride aqueous solution, the heat release reagent further comprises sodium silicate, and the mass ratio of the potassium chloride to the sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001-0.03); more specifically, the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001 to 0.01); in a specific embodiment, the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.002-0.008).
The heat release reagent provided by the application is mainly used for measuring the content of cadmium in soil to be 0.01-100 mg/kg, and under the condition, the mass ratio of potassium chloride to cadmium in soil is (5-200): (0.00001 to 1).
The application also provides a specific using method of the heat release reagent, which comprises the following steps:
paving a pyroelectric reagent at the bottom of a loading part, placing a soil sample on the surface of the pyroelectric reagent, placing the loading part on a sample introduction part of a detection instrument, and starting testing; the heat releasing reagent is potassium chloride particles;
or, dripping the heat releasing reagent on the soil sample of the loading part to enable the heat releasing reagent to fully infiltrate the soil sample, then placing the loading part on a sample introduction part of the detection instrument, and starting the test; the heat releasing reagent comprises a saturated potassium chloride aqueous solution;
or, placing the pyroelectric reagent in a loading part, drying and sealing to obtain the modified pyroelectric reagent, and starting testing; the pyroelectric reagent comprises a saturated aqueous solution of potassium chloride.
During the use of the thermolytic reagent, the AA2288 fully automatic cadmium tester, which is disclosed in the patent with the publication number CN110579564A, is mainly used for testing cadmium in soil. In the above-described method of use, the loading member is specifically selected from a sample boat; the analysis wavelength of the full-automatic cadmium detector is 228.8nm, the lamp current is 5.0mA, the negative high voltage of the PMT is-360V, and the atomizer is hydrogen flame.
The effective component of the thermolysis reagent for analyzing cadmium in soil provided by the invention is potassium chloride, and other components can improve the contact probability of potassium chloride and soil and fully play the role of potassium chloride.
For further understanding of the present invention, the thermolysis reagent for analyzing cadmium in soil and the method for using the same provided by the present invention are described in detail below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Examples
A) The formula of the effective heat release reagent is as follows:
formula 1: adding oxalic acid and quartz sand solid into potassium chloride solid, wherein the mass ratio of the oxalic acid to the quartz sand solid is (0.01-0.3) to (0.01-0.1): 1, fully and uniformly mixing; the oxalic acid is superior pure, and the cadmium content of the oxalic acid is lower than 0.0001 mg/kg; the quartz sand is 300-1000 mesh quartz sand powder, and the cadmium content of the quartz sand is lower than 0.0001 mg/kg; the potassium chloride is superior pure, and the cadmium content is lower than 0.0001 mg/kg. The three materials are fully stirred uniformly by a traditional Chinese medicine grinder, are in a uniform white powder or yellowish powder state, are easy to absorb moisture, and are stored in a sealed and light-proof way.
And (2) formula: adding oxalic acid solid and sodium silicate solid into saturated potassium chloride water solution according to the mass ratio range of (0.01-0.3) to (0.001-0.01): 1, fully shaking up; the oxalic acid is superior pure, and the cadmium content of the oxalic acid is lower than 0.0001 mg/kg; the sodium silicate is high-grade pure, and the cadmium content of the sodium silicate is lower than 0.0001 mg/kg; the potassium chloride is superior pure, and the cadmium content of the potassium chloride is lower than 0.0001 mg/kg; the water used was laboratory deionized water. The components are fully shaken up and then are placed in a polyethylene bottle with a cover for storage.
And (3) formula: potassium chloride granules; the potassium chloride is superior pure, and the cadmium content is lower than 0.0001 mg/kg.
And (4) formula: adding saturated potassium chloride water solution, adding sodium silicate, and mixing. The mass ratio of the solutes is within 1 (0.001-0.01), the potassium chloride is high-grade pure, and the cadmium content is lower than 0.0001 mg/kg; the water used was laboratory deionized water; the sodium silicate is superior pure, and the cadmium content of the sodium silicate is lower than 0.0001 mg/kg. After fully shaking up, the mixture is placed in a polyethylene bottle with a cover for storage.
In this embodiment, formula 1 specifically includes: the mass ratio of oxalic acid to quartz sand to potassium chloride is 0.1: 0.2: 1; the formula 2 specifically comprises: adding 10g of oxalic acid solid and 0.1g of sodium silicate solid into a saturated potassium chloride solution (36 g of potassium chloride); the formula 4 specifically comprises: 0.1g of sodium silicate solid was added to a saturated potassium chloride solution (36 g of potassium chloride).
B) The atomic absorption cadmium detector comprises the following instrument conditions and method procedures: (conditions of the apparatus corresponding to the cadmium tester when in use)
An instrument designed by adopting an electric heating evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method (application number 201911038388.3) is an AA2288 full-automatic cadmium measuring instrument, the instrument conditions are shown in table 1, and the method program design is shown in table 2;
TABLE 1 conditions of main parameters of cadmium tester
| Analyzing wavelength | 228.8nm |
| Lamp current | 5.0mA |
| Negative high pressure of PMT | -360V |
| Atomizer | Hydrogen flame |
Table 2 analytical methods reference procedure
C) Method of using a pyroelectric reagent
1) Formula 1, formula 3: spreading 0.1g (+ -0.01 g) of pyroelectric reagent on the bottom of the sample boat, then placing the soil sample on the pyroelectric reagent, placing the sample boat on an automatic sample injector part of an instrument, and clicking to start measurement;
2) formula 2, formula 4: dripping 0.05mL (+ -0.02 mL) of the pyroelectric reagent on a sample weighed in the sample boat to enable the pyroelectric reagent to completely soak the sample, placing the sample boat in an automatic sample injector part of an instrument, and clicking to start measurement;
3) other effective methods of use of the formulation: and (3) taking 0.2mL of the pyroelectric reagent corresponding to the formula 2 or the formula 4, placing the pyroelectric reagent in the sample boat, drying the pyroelectric reagent in an oven at 80 ℃ for 4 hours, and sealing and storing to obtain the modified sample boat. The modified sample boat can be directly used for measuring cadmium, so that a user does not need to add a heat release reagent again in the whole sample making process;
the thermolysis design is modified for one time, and the next sample test can be carried out by adding the thermolysis reagent again after the cadmium in the soil sample is measured for one time.
D) The content of cadmium in the soil sample is detected by using the pyroelectric reagent in the formula 1,
as shown in table 3, table 3 is a table of test effect data of cadmium in the soil sample obtained before and after the addition of the pyroelectric reagent;
TABLE 3 test results of soil standard samples before and after adding pyroelectric reagent
Table 3 (next): test result table of soil standard sample before and after adding pyroelectric reagent
According to the analysis of the results counted in the table 3, the accuracy coincidence rate of the soil sample test is greatly improved from 37.9% to 96.6% before and after the heat release reagent is used, the relative error of the sample test is improved from-41.7% to-2.8% at the maximum, the recovery rate of cadmium in the sample is greatly improved, the stable superiority of the parallel sample test is not damaged, and the phenomenon that the cadmium in the sample is tested to be low is completely solved.
E) Comparison of sample signal peaks before and after addition of pyroelectric reagent
In order to more intuitively obtain the effectiveness of the pyroelectric reagent, fig. 1 is a comparison graph of peak patterns before and after the pyroelectric reagent of formula 1 is added to a soil sample; FIG. 1-a depicts the change of sample signal before and after adding a matrix effect significant sample thermolytic agent, wherein the dashed peak is the cadmium signal peak obtained by the soil sample (GSS-40) when the agent is not heated and the solid peak is the cadmium signal peak obtained by adding the thermolytic agent to the soil sample (GSS-40) of the same mass, as is apparent from the figure, the use of the thermolytic agent significantly improves the signal response of cadmium; fig. 1-b illustrates a soil sample without matrix effect (i.e. the accuracy of the test of the unheated released reagent is also a sample meeting the requirement), wherein the dotted line peak is the cadmium signal peak obtained by the soil sample (GSS-39) when the unheated released reagent is released, and the solid line peak is the cadmium signal peak obtained by the soil sample (GSS-39) with the same mass after the heat release reagent is added, so that the sample without matrix effect is not interfered after the heat release reagent is added.
F) Detecting the content of cadmium in soil by adopting different formulas
In order to fully illustrate the effectiveness of other formula reagents, the formulas 1, 2, 3 and 4 are respectively used as heat release reagents, the electric heating evaporation (heating quartz tube), hydrogen flame atomization and atomic absorption method (application number 201911038388.3) is used for analyzing cadmium in a batch of farmland soil samples and soil samples of construction land, and the national standard method (graphite furnace atomic absorption method GF-AAS: GB/T17141) is used for carrying out fixed value analysis on cadmium in the soil samples.
The results measured before and after the heat release agent is added are compared with the results measured by the GF-AAS method, the analysis results are shown in figure 2, figure 2 is an analysis graph of the results measured before and after the 4 kinds of heat release agents are added and the results measured by the GF-AAS method, the dotted line shows the content of cadmium in 15 soil samples measured by adopting an electrothermal evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method without heating the release agents, the dark black is the content of cadmium in the soil measured by adopting a national standard analysis method (GF-AAS), and the rest are the results used in the electrothermal evaporation (heating quartz tube) -hydrogen flame atomization-atomic absorption method by using the formula 1, the formula 2, the formula 3 and the formula 4 in sequence. As can be seen from fig. 2, all of the pyroelectric reagent formulas 1, 2, 3 and 4 can effectively improve the recovery rate of cadmium, and the measured value of cadmium is consistent with that measured by the national standard method, which indicates that all of the pyroelectric reagents of these 4 formulas are effective.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The heat releasing reagent for analyzing cadmium in soil includes potassium chloride, which is potassium chloride particle or saturated potassium chloride aqua.
2. The pyroelectric reagent as claimed in claim 1, wherein when the potassium chloride is potassium chloride particles, the pyroelectric reagent further comprises oxalic acid and quartz sand; the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.5): (0.01-0.3): 1.
3. the pyroelectric reagent according to claim 2, characterized in that the mass ratio of the oxalic acid to the quartz sand to the potassium chloride is (0.01-0.3): (0.01-0.1): 1.
4. the pyroelectric reagent as claimed in claim 1, wherein when the potassium chloride is a saturated potassium chloride aqueous solution, the pyroelectric reagent further comprises oxalic acid and sodium silicate, and the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.5): (0.001-0.03): 1.
5. the pyroelectric reagent as claimed in claim 4, wherein the mass ratio of the oxalic acid to the sodium silicate to the potassium chloride in the saturated potassium chloride aqueous solution is (0.01-0.3): (0.001-0.01): 1.
6. the pyroelectric reagent as claimed in claim 1, wherein when the potassium chloride is a saturated potassium chloride aqueous solution, the pyroelectric reagent further comprises sodium silicate, and the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001-0.03).
7. The pyroelectric reagent as claimed in claim 6, wherein the mass ratio of potassium chloride to sodium silicate in the saturated potassium chloride aqueous solution is 1: (0.001-0.01).
8. The pyroelectric reagent as claimed in claim 1, wherein the content of cadmium in the soil is 0.01-100 mg/kg, and the mass ratio of the potassium chloride to the cadmium in the soil is (5-200): (0.00001 to 1).
9. The method of using the pyro-releasing agent of any one of claims 1 to 8, comprising:
paving a pyroelectric reagent at the bottom of a loading part, placing a soil sample on the surface of the pyroelectric reagent, placing the loading part on a sample introduction part of a detection instrument, and starting testing; the pyroelectric reagent comprises potassium chloride particles;
or, dripping the heat releasing reagent on the soil sample of the loading part to enable the heat releasing reagent to fully infiltrate the soil sample, then placing the loading part on a sample introduction part of the detection instrument, and starting the test; the heat releasing reagent comprises a saturated potassium chloride aqueous solution;
or, the pyroelectric reagent is placed in a loading part, dried and sealed to obtain a modified pyroelectric reagent loading part which is used as a disposable modified loading part; the disposable modified loading component can directly weigh a soil sample to start testing; the pyroelectric reagent comprises a saturated aqueous solution of potassium chloride.
10. The use method of claim 9, wherein the detection instrument is an AA2288 fully automatic cadmium detector; the analysis wavelength of the full-automatic cadmium detector is 228.8nm, the lamp current is 5.0mA, the negative high voltage of the PMT is-360V, and the atomizer is hydrogen flame; the detecting step comprises drying, temperature rising, pyrolysis and gas switching.
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