CN113720828A - Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method - Google Patents
Method for determining phosphorus and sulfur in fresh plant sample by microwave digestion-ICP-AES (inductively coupled plasma-atomic emission Spectrometry) method Download PDFInfo
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- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 73
- 239000011574 phosphorus Substances 0.000 title claims abstract description 73
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 72
- 239000011593 sulfur Substances 0.000 title claims abstract description 72
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 56
- 230000029087 digestion Effects 0.000 claims abstract description 50
- 230000004044 response Effects 0.000 claims abstract description 25
- 239000000523 sample Substances 0.000 claims description 86
- 241000196324 Embryophyta Species 0.000 claims description 67
- 239000012086 standard solution Substances 0.000 claims description 44
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 24
- 239000012496 blank sample Substances 0.000 claims description 24
- 229910017604 nitric acid Inorganic materials 0.000 claims description 24
- 238000000120 microwave digestion Methods 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 240000007087 Apium graveolens Species 0.000 claims description 7
- 235000015849 Apium graveolens Dulce Group Nutrition 0.000 claims description 7
- 235000010591 Appio Nutrition 0.000 claims description 7
- 244000036905 Benincasa cerifera Species 0.000 claims description 7
- 235000011274 Benincasa cerifera Nutrition 0.000 claims description 7
- 235000010149 Brassica rapa subsp chinensis Nutrition 0.000 claims description 7
- 235000000536 Brassica rapa subsp pekinensis Nutrition 0.000 claims description 7
- 241000499436 Brassica rapa subsp. pekinensis Species 0.000 claims description 7
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 claims description 7
- 244000061456 Solanum tuberosum Species 0.000 claims description 7
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 150000003017 phosphorus Chemical class 0.000 claims description 6
- 150000003463 sulfur Chemical class 0.000 claims description 6
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000010354 integration Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 244000241257 Cucumis melo Species 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 17
- 238000004737 colorimetric analysis Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 241000219112 Cucumis Species 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 239000003517 fume Substances 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 238000004993 emission spectroscopy Methods 0.000 description 3
- 235000012015 potatoes Nutrition 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
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- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000020774 essential nutrients Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
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- 239000002245 particle Substances 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000012791 spiking procedure Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention relates to the technical field of chemical detection, and provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps: drawing a standard curve of the phosphorus and sulfur solution; digesting a fresh plant sample; the digestion sample is used for measuring the element response value through an ICP-AES instrument; and finally obtaining the mass concentrations of phosphorus and sulfur in the fresh plant sample. The digestion method solves the problems that in the prior art, a plant sample needs to be dried or air-dried in advance, interference cannot be eliminated in the determination of the inductively coupled plasma mass spectrometry, and the colorimetric method is complicated, directly uses a fresh plant sample for digestion, avoids secondary pollution to the sample in the drying process, reduces detection steps by using the ICP-AES method, and greatly shortens the detection time.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method.
Background
Phosphorus is an essential nutrient element in plants, and mainly influences the processes of photosynthesis, respiration, biosynthesis and the like in plants, and the morphological and physiological changes of the plants are caused by the lack of phosphorus in the plants. Sulfur is an important nutrient element of plants, mainly participates in the synthesis of various chemical compounds in the plants, and is a main regulating element for the metabolism of the plants. The functions of phosphorus and sulfur in plants and the absorption amount of crops to the phosphorus and sulfur are very similar, so that the rapid determination of the phosphorus and the sulfur in the plants is of great significance.
The pretreatment methods of phosphorus and sulfur in plants mainly comprise a dry ashing method, a wet open digestion method, a wet closed digestion method, a microwave digestion method and the like, wherein the dry ashing method easily causes the loss of phosphorus and sulfur in a sample in the combustion process and easily causes the mutual pollution of the sample; the acid amount for wet-process open digestion is relatively large, the digestion efficiency is relatively poor, and interactive pollution is easily caused; the wet closed digestion and digestion time is too long; the microwave digestion method has short digestion time, small acid consumption and difficult pollution.
The method for detecting phosphorus and sulfur in the plant sample mainly comprises a colorimetric method, an inductively coupled plasma emission spectrometry, an inductively coupled plasma mass spectrometry and the like. The colorimetric method has long color reaction time, is easy to be interfered by pigments, particularly for plant samples which are difficult to digest, the interference is more serious in the color development process, and simultaneously, the colorimetric method can only detect one element at a time; interference exists in the inductively coupled plasma mass spectrometry, and deviation is easy to occur in the detection result of a high-content sample; by utilizing the inductively coupled plasma emission spectrometry, the interference of pigments can be avoided, phosphorus and sulfur elements in the plant sample can be simultaneously digested, the sample with higher content can be detected, and the sample detection time is greatly shortened. However, the existing methods are all to measure dry plants, and the cleaned plant samples need to be dried or air-dried and then digested. Therefore, the research determines an optimal digestion method by selecting microwave digestion conditions, directly weighs a fresh plant sample for digestion, selects an optimal spectral line on an inductively coupled plasma emission spectrometer, determines phosphorus and sulfur in the plant, reduces secondary pollution and improves detection speed.
Disclosure of Invention
The invention aims to provide a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which can effectively reduce secondary pollution caused by the drying process of the plant sample and directly weigh the fresh plant sample for digestion so as to greatly shorten the detection time. Meanwhile, the ICP-AES method is used for replacing the traditional method, so that the detection steps are reduced.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) mixing fresh plants, concentrated nitric acid and hydrogen peroxide solution, and then digesting to obtain a digested sample;
concentrated nitric acid is used as a blank sample;
(3) determining the volume of the digestion sample, and measuring element response values of the digestion sample and the blank sample by an ICP-AES instrument;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur elements in the digestion sample and the blank sample, and finally obtaining the mass concentrations of phosphorus and sulfur in the fresh plant sample.
Preferably, in the step (2), the fresh plants are Chinese cabbages, celery, white gourds, melons or potatoes, and the weight of the fresh plants is 2.0000-3.0000 g.
Preferably, the feed-liquid ratio of the fresh plants to the concentrated nitric acid in the step (2) is 2-3 g: 5-10 mL, and the concentration of the concentrated nitric acid is 60-75%.
Preferably, the feed-liquid ratio of the fresh plants to the hydrogen peroxide solution in the step (2) is 2-3 g: 0.5-3 mL, and the concentration of the hydrogen peroxide solution is 20-40%.
Preferably, the hydrogen peroxide solution is added after the fresh sample reacts with the concentrated nitric acid for 5-20 min in the step (2).
Preferably, the digestion in the step (2) is microwave digestion, and the microwave digestion processing program specifically comprises:
heating to the initial temperature of 130-150 ℃ for 2-8 min, keeping the temperature for 5-15 min, and keeping the power of 500-1000W;
heating to 150-190 ℃ in 2-8 min, keeping the temperature for 2-10 min, and keeping the power at 1000-1500W;
heating to 180-220 ℃ for 1-5 min, keeping the temperature for 5-15 min, and keeping the power at 1500-2000W;
cooling to below 40 ℃ in 5-15 min, and the power is 500-1000W.
Preferably, the measurement conditions of the ICP-AES instrument in the step (3) are as follows:
1) the radio frequency power is 1100-1200W;
2) the auxiliary gas flow is 0.5-0.8L/min;
3) the gas flow of the atomizer is 0.7-1.3L/min;
4) the vertical observation height is 10-15 mm;
5) measuring for 2-5 times;
6) the speed of the washing pump is 50-100 r/min;
7) analyzing the pump speed of 30-100 r/min;
8) sample introduction and washing time is 10-20 s;
9) the exposure time is in a low wave range of 3-10 s and in a high wave range of 8-15 s;
10) the maximum integration time is 20-30 s.
The invention has the technical effects and advantages that:
the invention provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, wherein the digestion step in the method can effectively reduce secondary pollution caused by the drying process of the plant sample, and the fresh plant sample is directly weighed for digestion, so that the detection time is greatly shortened; the ICP-AES method is used for directly detecting the fresh sample, and meanwhile, the water content is measured, so that the detection efficiency of the sample is improved, the generation of secondary pollution is reduced, and the detection steps are reduced.
Detailed Description
The invention provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) mixing fresh plants, concentrated nitric acid and hydrogen peroxide solution, and then digesting to obtain a digested sample;
concentrated nitric acid is used as a blank sample;
(3) determining the volume of the digestion sample, and measuring element response values of the digestion sample and the blank sample by an ICP-AES instrument;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur elements in the digestion sample and the blank sample, and finally obtaining the mass concentrations of phosphorus and sulfur in the fresh plant sample.
The fresh plants are preferably Chinese cabbages, celery, wax gourds, melons or potatoes, more preferably Chinese cabbages, celery, wax gourds, melons or potatoes with the water content of more than 50%, and the weight is preferably 2.0000-3.0000 g, and more preferably 2.2500-2.7500 g.
The feed-liquid ratio of the fresh plants to the concentrated nitric acid is preferably 2-3 g: 5-10 mL, more preferably 2.25-2.75 g: 6-8 mL, and the concentration of the concentrated nitric acid is preferably 60-75%, more preferably 65-70%.
The feed-liquid ratio of the fresh plants to the hydrogen peroxide solution is preferably 2-3 g: 0.5-3 mL, more preferably 2.25-2.75 g: 1-2 mL, and the concentration of the hydrogen peroxide solution is preferably 20-40%, more preferably 25-35%.
In the invention, a fresh sample and concentrated nitric acid are placed in a fume hood for pre-reaction and then added with a hydrogen peroxide solution, the nitric acid has a pre-digestion effect on the sample, the sample with a larger volume can be digested into a small volume, or the internal structure of sample particles is damaged, and the sample subjected to the pre-digestion by the nitric acid is added with the hydrogen peroxide solution, so that the digestion speed is higher and the digestion is more thorough when the microwave digestion is carried out; in addition, the hydrogen peroxide solution is digested with plants to generate a large amount of bubbles, and the bubbles overflow if the hydrogen peroxide solution is added in advance.
The reaction time of the fresh sample and the concentrated nitric acid is preferably 5-20 min, and more preferably 10-15 min.
The digestion is preferably microwave digestion, and the microwave digestion treatment program is preferably as follows:
heating to the initial temperature of 130-150 ℃ for 2-8 min, keeping the temperature for 5-15 min, and keeping the power of 500-1000W;
heating to 150-190 ℃ in 2-8 min, keeping the temperature for 2-10 min, and keeping the power at 1000-1500W;
heating to 180-220 ℃ for 1-5 min, keeping the temperature for 5-15 min, and keeping the power at 1500-2000W;
cooling to below 40 ℃ in 5-15 min, and the power is 500-1000W;
more preferably:
heating to the initial temperature of 135-145 ℃ for 4-7 min, keeping the temperature for 8-12 min, and keeping the power of 600-800W;
heating to 160-180 ℃ in 3-6 min, keeping the temperature for 4-8 min, and keeping the power at 1100-1300W;
heating to 190-210 ℃ in 2-4 min, keeping the temperature for 8-12 min, and keeping the power at 1600-1900W;
cooling to below 20 ℃ in 8-12 min, and the power is 600-800W.
The measurement conditions of the ICP-AES instrument are preferably as follows:
1) the radio frequency power is 1100-1200W;
2) the auxiliary gas flow is 0.5-0.8L/min;
3) the gas flow of the atomizer is 0.7-1.3L/min;
4) the vertical observation height is 10-15 mm;
5) measuring for 2-5 times;
6) the speed of the washing pump is 50-100 r/min;
7) analyzing the pump speed of 30-100 r/min;
8) sample introduction and washing time is 10-20 s;
9) the exposure time is in a low wave range of 3-10 s and in a high wave range of 8-15 s;
10) the maximum integration time is 20-30 s;
more preferably:
1) the radio frequency power is 1150-1180W;
2) the auxiliary gas flow is 0.6-0.7L/min;
3) the gas flow of the atomizer is 0.8-1.2L/min;
4) the vertical observation height is 12-14 mm;
5) measuring for 3-4 times;
6) the speed of the washing pump is 60-80 r/min;
7) analyzing the pump speed of 50-80 r/min;
8) the sample introduction and washing time is 12-18 s;
9) the exposure time is in a low wave range of 5-8 s and in a high wave range of 10-12 s;
10) the maximum integration time is 24-26 s.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) selecting plant samples of Weinan Shaanxi and Ganxi, wherein the fresh plant samples mainly comprise Chinese cabbage, celery, wax gourd, melon and potato, weighing 2.5000g of the fresh samples in a microwave digestion tank, adding 6mL of concentrated nitric acid (premium grade purity, 68%), placing the fresh samples in a fume hood for 10 minutes, then adding 1mL of hydrogen peroxide solution (premium grade purity) with the volume fraction of 30%, adjusting a microwave digestion program, wherein the microwave digestion program is specifically shown in Table 1, and completely digesting the samples in a microwave digestion instrument;
(3) and (4) fixing the volume of the digestion sample to a 50mL colorimetric tube by using pure water, and fully shaking up for later use. Taking concentrated nitric acid as a blank sample, passing the digestion sample and the blank sample through an ICP-AES instrument, wherein the measurement conditions of the ICP-AES instrument are shown in Table 2, and measuring the element response values of the digestion sample and the blank sample;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur in the digestion sample and the blank sample,
according to the formula: w ═ C-C0 (Ci) x V/m
In the formula: w represents the mass fraction (mg/kg) of phosphorus and sulfur in the sample;
ci-mass concentration (mg/kg) of phosphorus and sulfur elements in the digestion sample;
c0 mass concentration (mg/kg) of phosphorus and sulfur in blank sample;
v-digestion sample volume (mL);
m-weighing the mass (g) of a fresh sample;
the contents of phosphorus and sulfur in the fresh plant samples can be calculated.
TABLE 1 optimized post microwave digestion procedure
TABLE 2 optimized ICP-AES Instrument conditions
Example 2
The embodiment provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) selecting plant samples of Weinan Shaanxi and Ganxi, wherein the fresh plant samples mainly comprise Chinese cabbage, celery, wax gourd, melon and potato, weighing 2.2500g of the fresh samples in a microwave digestion tank, adding 7mL of concentrated nitric acid (premium grade purity, 65%), placing in a fume hood for more than 20 minutes, then adding 1.5mL of hydrogen peroxide solution (premium grade purity) with the volume fraction of 25%, adjusting a microwave digestion program, wherein the microwave digestion program is specifically shown in Table 3, and completely digesting the samples in a microwave digestion instrument;
(3) and (4) fixing the volume of the digestion sample to a 50mL colorimetric tube by using pure water, and fully shaking up for later use. Taking concentrated nitric acid as a blank sample, passing the digestion sample and the blank sample through an ICP-AES instrument, wherein the measurement conditions of the ICP-AES instrument are shown in Table 4, and measuring the element response values of the digestion sample and the blank sample;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur in the digestion sample and the blank sample,
according to the formula: w ═ C-C0 (Ci) x V/m
In the formula: w represents the mass fraction (mg/kg) of phosphorus and sulfur in the sample;
ci-mass concentration (mg/kg) of phosphorus and sulfur elements in the digestion sample;
c0 mass concentration (mg/kg) of phosphorus and sulfur in blank sample;
v-digestion sample volume (mL);
m-weighing the mass (g) of a fresh sample;
the contents of phosphorus and sulfur in the fresh plant samples can be calculated.
TABLE 3 optimized post microwave digestion procedure
TABLE 4 Instrument conditions of ICP-AES after optimization
Example 3
The embodiment provides a method for determining phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method, which comprises the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) selecting plant samples of Weinan Shaanxi and Ganxi, wherein the fresh plant samples mainly comprise Chinese cabbage, celery, wax gourd, melon and potato, weighing 2.7500g of the fresh samples in a microwave digestion tank, adding 8mL of concentrated nitric acid (superior purity, 70%), placing in a fume hood for more than 15 minutes, then adding 2mL of hydrogen peroxide solution (superior purity) with the volume fraction of 35%, adjusting the microwave digestion program, wherein the microwave digestion program is specifically shown in Table 5, and completely digesting the samples in a microwave digestion instrument;
(3) and (4) fixing the volume of the digestion sample to a 50mL colorimetric tube by using pure water, and fully shaking up for later use. Taking concentrated nitric acid as a blank sample, passing the digestion sample and the blank sample through an ICP-AES instrument, wherein the measurement conditions of the ICP-AES instrument are shown in Table 6, and measuring the element response values of the digestion sample and the blank sample;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur in the digestion sample and the blank sample,
according to the formula: w ═ C-C0 (Ci) x V/m
In the formula: w represents the mass fraction (mg/kg) of phosphorus and sulfur in the sample;
ci-mass concentration (mg/kg) of phosphorus and sulfur elements in the digestion sample;
c0 mass concentration (mg/kg) of phosphorus and sulfur in blank sample;
v-digestion sample volume (mL);
m-weighing the mass (g) of a fresh sample;
the contents of phosphorus and sulfur in the fresh plant samples can be calculated.
TABLE 5 optimized post microwave digestion procedure
TABLE 6 optimized ICP-AES Instrument conditions
Sample recovery was determined according to the assay of example 1, the spiking procedure: taking two fresh plant samples, adding a commercially available standard solution (GBW (E)083181-1, GBW (E) 082688-4) of elements to be detected into one fresh plant sample, wherein the concentrations of phosphorus and sulfur are 1000mg/L, Beijing Tan ink quality testing science and technology Co., Ltd.), and determining the specific addition amount of the standard solution according to the contents of phosphorus and sulfur in plants. After treatment according to the experimental method of example 1, the analysis was carried out under optimized experimental conditions. The analysis results obtained are shown in Table 7.
TABLE 7 analysis results of various kinds of fresh samples
Phosphorus and sulfur elements in the plant sample are measured by using a microwave digestion-inductively coupled plasma emission spectrometry, a fresh sample is subjected to a standard addition test by optimizing a digestion method and a detection method, the recovery rate is between 90.5 and 107 percent, and the results show that the fresh plant sample can be directly used for digestion measurement, and the results meet the detection requirements of the plant sample in the technical requirements for analysis and supplement of ecological geochemistry evaluation samples (DD 2005-03).
According to the embodiment, the invention provides the method for determining phosphorus and sulfur in the fresh plant sample by the microwave digestion-ICP-AES method, the digestion step in the method can effectively reduce secondary pollution caused by the drying process of the plant sample, and the fresh plant sample is directly weighed for digestion, so that the detection time is greatly shortened; the ICP-AES method is used for directly detecting the fresh sample, and meanwhile, the water content is measured, so that the detection efficiency of the sample is improved, the generation of secondary pollution is reduced, and the detection steps are reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A method for measuring phosphorus and sulfur in a fresh plant sample by a microwave digestion-ICP-AES method is characterized by comprising the following steps:
(1) preparing a series of phosphorus element standard solutions with increasing concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission spectrometry) determination on the standard solutions, and drawing a phosphorus element standard solution curve by taking the phosphorus element concentration as a horizontal coordinate and the determined phosphorus element response value as a vertical coordinate;
preparing a series of sulfur element standard solutions with gradually increased concentrations, sequentially carrying out ICP-AES (inductively coupled plasma-atomic emission Spectrometry) determination on the standard solutions, and drawing a sulfur element standard solution curve by taking the sulfur element concentration as a horizontal coordinate and the determined sulfur element response value as a vertical coordinate;
(2) mixing fresh plants, concentrated nitric acid and hydrogen peroxide solution, and then digesting to obtain a digested sample;
concentrated nitric acid is used as a blank sample;
(3) determining the volume of the digestion sample, and measuring element response values of the digestion sample and the blank sample by an ICP-AES instrument;
(4) substituting the element response values into the standard solution curve to obtain the mass concentrations of phosphorus and sulfur elements in the digestion sample and the blank sample, and finally obtaining the mass concentrations of phosphorus and sulfur in the fresh plant sample.
2. The method according to claim 1, wherein the fresh plant in the step (2) is Chinese cabbage, celery, wax gourd, melon or potato, and the weight of the fresh plant is 2.0000-3.0000 g.
3. The method according to claim 1, wherein the feed-to-liquid ratio of the fresh plants to the concentrated nitric acid in the step (2) is 2-3 g: 5-10 mL, and the concentration of the concentrated nitric acid is 60-75%.
4. The method according to claim 1, wherein the feed-to-liquid ratio of the fresh plants to the hydrogen peroxide solution in the step (2) is 2-3 g: 0.5-3 mL, and the concentration of the hydrogen peroxide solution is 20-40%.
5. The method according to claim 1, wherein the hydrogen peroxide solution is added after the fresh sample reacts with the concentrated nitric acid for 5-20 min in the step (2).
6. The method according to any one of claims 1 to 5, wherein the digestion in the step (2) is microwave digestion, and the microwave digestion processing program is specifically as follows:
heating to the initial temperature of 130-150 ℃ for 2-8 min, keeping the temperature for 5-15 min, and keeping the power of 500-1000W;
heating to 150-190 ℃ in 2-8 min, keeping the temperature for 2-10 min, and keeping the power at 1000-1500W;
heating to 180-220 ℃ for 1-5 min, keeping the temperature for 5-15 min, and keeping the power at 1500-2000W;
cooling to below 40 ℃ in 5-15 min, and the power is 500-1000W.
7. The method according to claim 1, wherein the ICP-AES instrument determination conditions in step (3) are as follows:
1) the radio frequency power is 1100-1200W;
2) the auxiliary gas flow is 0.5-0.8L/min;
3) the gas flow of the atomizer is 0.7-1.3L/min;
4) the vertical observation height is 10-15 mm;
5) measuring for 2-5 times;
6) the speed of the washing pump is 50-100 r/min;
7) analyzing the pump speed of 30-100 r/min;
8) sample introduction and washing time is 10-20 s;
9) the exposure time is in a low wave range of 3-10 s and in a high wave range of 8-15 s;
10) the maximum integration time is 20-30 s.
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