CN103063641A - Method for determining arsenic content of plants - Google Patents
Method for determining arsenic content of plants Download PDFInfo
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- CN103063641A CN103063641A CN2012105922660A CN201210592266A CN103063641A CN 103063641 A CN103063641 A CN 103063641A CN 2012105922660 A CN2012105922660 A CN 2012105922660A CN 201210592266 A CN201210592266 A CN 201210592266A CN 103063641 A CN103063641 A CN 103063641A
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Abstract
The invention discloses a method for determining the arsenic content of plants. The detection process of the method comprises the following steps: weighing 0.5g of plant sample sieved by 100 meshes, putting into a 50mL glass colorimetric tube with scales and a stopper, adding 35mL of concentrated nitric acid HNO, capping and immersing for the night, and meanwhile doing a reagent blank without samples; the next day, heating and digestion for 2 hours with a water bath at 100 DGE C; after heating and digestion are finished, putting a Vapor Block, and evaporating nitric acid to be dry at 120-130 DEG C; after catching acid is finished, taking down the colorimetric tube, cooling, adding 5mL of hydrochloric acid and 5mL of mixed liquid of 50g/L thiourea and 50g/L ascorbic acid, and adding ultrapure water to cause the constant volume to be 25mL; and after filtering, using an atomic fluorescence analyzer to determine the arsenic content. Compared with the traditional method for determining the arsenic content, the method has the beneficial effects that the advantages are significant, and the detection speed is high; the plant samples can be processed in batches, the practicality of nitric acid is greatly reduced, less nitrogen oxide waste gas is generated, and the environmental pollution is greatly reduced; and the detection result of the method has high accuracy and good repeatability.
Description
Technical field
The present invention relates to a kind of mensuration content field, more specifically, it relates to the assay method of arsenic content in the Plants.
Background technology
Soil is the material base that the mankind depend on for existence, is the important component part of human ecological environment.Yet because a large amount of dischargings of three industrial wastes, and the using in a large number of agricultural chemicals, chemical fertilizer, arsenic in soil pollutes and is on the rise, and it directly causes soil degradation, and yield-power descends and then the health of harm humans.Arsenic is distributed widely in natural air, the water and soil.The excessive arsenic of accumulation can suppress the growth of soil microorganism, the activity of soil enzyme in the soil, and then affects the physiological metabolism of plant, is subjected to the soil of arsenic contamination can pass through the final harm humans health of the media such as water, plant.The method and the technology that are used for the pollution of removing arsenic in soil are a lot, common are to change the cultivation management system, and washing soil applies antagonist, modifying agent in soil, and phytoremediation and microorganism are repaired, multiple reparation is combined with etc.Though each tool advantage of these methods is temporary transient fixing to arsenic, also may cause secondary pollution, can not fundamentally solve the arsenic contamination problem.And phytoremediation technology exactly has above irreplaceable advantage as a kind of original position reparation, shows as permanent, the original position (little to the soil environment disturbance) of governance process of regulation effect, the cheap property for the treatment of cost, the compatibility of the aesthetics of environment, the characteristics such as simplification of post-processed.Therefore, utilize plant As polluted soil reparation to be become the study hotspot in present reparation field.Phytoremediation has broad application prospects as the pollution remediation technology of a kind of " green ".But it also requires further study in the As polluted soil and explores being applied to administer.The Treatment and recovery utilization in postpartum of the super accumulation of arsenic plant is important link in the phytoremediation.Behind the results rehabilitation plant of planting, if it is arbitrarily abandoned, can cause to environment " secondary pollution " like this, it is carried out arsenic content and recovery is key and the difficult point of the accumulation of plant soil restoration arsenic.Both at home and abroad to Pb, it is more that the super accumulation of zn and Cu phytoremediation disposal technology in postpartum is studied, and generally mostly is burning method, composting process, compression landfill method, high-temperature decomposition, liquid-phase extraction method etc., but less to the research of arsenic at present.Should seek the detection in postpartum of the super accumulation of a kind of efficient arsenic plant, treatment technology for this reason, really pollutant forever be removed, realize simultaneously the purpose of " turning waste into wealth ".
In the existing technology, atomic fluorometry is the Main Means of environmental sample arsenic content analysis because easy and simple to handle, highly sensitive, collective disturbs less, analysis result is stable.The pre-treatment of atomic fluorescence method and testing process are: get a certain amount of disappearing and boil rear sample, the mixed liquor that adds hydrochloric acid and thiocarbamide and ascorbic acid is behind the mixing, take potassium borohydride as reductive agent, 5%HCl is current-carrying, adopts the content of Hydrides AFS spectrophotometer arsenic.The effect that adds thiocarbamide in the testing sample is mainly used to shelter the Cu of constant in the sample and a small amount of Ni, Co ion etc., determines that through testing 1% thiourea concentration can guarantee quantitatively to shelter whole Cu ions.When the concentration of HCl in the sample during greater than 2.5mL/L, thiocarbamide can also play the reductive agent effect, and pentavalent arsenic is reduced to trivalent.The effect of ascorbic acid is to reduce in advance pentavalent arsenic to trivalent, to guarantee the complete of next step hydrogenation.The principle of work of Hydrides AFS spectrometer is, under acid condition, take potassium borohydride as reductive agent, make arsenic generate arsenic hydride, being written into the quartz atomizer decomposes by carrier gas (argon gas) is atomic state arsenic, under the radiative irradiation of special as hollow cathode lamp, ground state arsenic atom is excited to high-energy state, launch the fluorescence of characteristic wavelength, its fluorescence intensity is directly proportional with arsenic content in the finite concentration scope, and is more quantitative with standard series.
2 kinds of the pre-treatment of atomic fluorometry heating board digestion commonly used and micro-wave digestions, 2 operations are all easier, but the former length consuming time, blank value is high, and produces a large amount of NO in the process of boiling that disappears
2, contaminated environment; And the acid of catching up with of sample has 2 kinds of methods behind latter's micro-wave digestion, adopt Vapor Block to catch up with sour device to catch up with acid or boil from disappearing the pipe sample transferred in the crucible and catch up with acid at electric hot plate, no matter adopt any method, in pilot process, all need to shift several times, affect the reference material recovery, and need to be equipped with microwave dissolver, experiment condition is higher.2 kinds of digestion processes all are not suitable for batch samples (40 sample/time more than) and detect in addition.The objective of the invention is provides a kind of detection speed fast by improving the pretreatment process of plant sample, can carry out mass disposal to plant sample, and environmental pollution is little, and the testing result accuracy is high, the assay method of arsenic content in the plant of good reproducibility.
Summary of the invention
Defective for prior art, the invention provides the assay method of arsenic content in the Plants, specifically adopt the digestion of boiling water bath wet method to measure the method for the arsenic content of plant in conjunction with atomic fluorometry, the method and traditional Spectrometric Determination Arsenic Content are relatively, advantage is remarkable, its detection speed is fast, can carry out mass disposal to plant sample, greatly reduce the practicality of nitric acid, produce less nitrogen dioxide waste gas, greatly reduce environmental pollution, and the accuracy of the method testing result is high, good reproducibility.
The objective of the invention is to be achieved through the following technical solutions.The assay method of arsenic content in this Plants adopts the immersion method sample digestion, the Hydrides AFS spectrophotometer, and its testing process: the plant sample 0.5g after taking by weighing 100 orders and sieving, place 50mL band scale tool plug glass color comparison tube, add red fuming nitric acid (RFNA) HNO
35mL adds a cover soaked overnight, does simultaneously the n.s. reagent blank; Disappear in 100 ℃ of water-baths and boil 2 hours next day, disappear boil end after, place Vapor Block to catch up with sour device, it is dried under 120 ℃ to 130 ℃ nitric acid to be evaporated to; After catching up with acid to finish, take off color comparison tube, cooling adds hydrochloric acid 5mL, 50g/L thiocarbamide+50g/L ascorbic acid mixed liquor 5mL, and ultrapure water is settled to 25mL, mixing, upper atomic fluorescence analysis instrument is measured arsenic content after filtering.
Described disappearing boiled sample and directly placed Vapor Block to catch up with sour device to catch up with acid in the glass color comparison tube.
Described water-bath process is to place two row, six hole electric-heated thermostatic water baths, once can sample digestion more than 70.
Zeeman GFAAS: adopt the Hydrides AFS spectrometer analysis, reductive agent is 1% potassium borohydride+0.2% potassium hydroxide, and 5%HCL is as current-carrying.
The invention has the beneficial effects as follows: the inventive method has been improved digestion process, adopts immersion method digestion, and equipment is simple, and required time is short, can realize the mass disposal to sample; The inventive method has also adopted Vapor Block to catch up with sour device directly the sample digestion in the glass color comparison tube to be caught up with acid, the transfer of therefore having omitted middle sample.And because the nitric acid amount that adds is less, the NO of generation
2Measure lessly, environmental pollution is few.
Embodiment
Below in conjunction with embodiment the present invention is described further.Although the present invention is described in connection with preferred embodiment, should know, do not represent to limit the invention among the described embodiment.On the contrary, the present invention will be contained alternative, modified and the equivalent in the scope of the present invention that can be included in attached claims restriction.
The plant sample preparation: the plant sample oven dry, cross 100 mesh sieves after pulverizing.
Treatments of the sample: take by weighing and ground 100 purpose plant sample 0.5g, place 50mL band scale tool plug glass color comparison tube, add the pure red fuming nitric acid (RFNA) 5mL of 5mL top grade, add a cover soaked overnight, do simultaneously the n.s. reagent blank.Next day, disappear in 100 ℃ of water-baths and to boil 2 hours.
Sample is caught up with acid: take out color comparison tube from water-bath, place Vapor Block to catch up with sour device, be evaporated to dried under 120 ℃ to 130 ℃.
Sample pretreatment: after catching up with acid to finish, take off color comparison tube, cooling adds hydrochloric acid 5mL, 50g/L thiocarbamide+50g/L ascorbic acid mixed liquor 5mL, and ultrapure water is settled to 25mL, and mixing filters.
Sample determination: adopt the Hydrides AFS spectrometer analysis, reductive agent is 1% potassium borohydride+0.2% potassium hydroxide, and 5%HCL is as current-carrying.
Instrument condition of work: lamp current 65mA; PMT 200V; Atomizer: room temperature; Atomization mode: flame method; Carrier gas: 900mL/min.
To plant standard substance GSV-1 and the Chinese cabbage of picking up from Beijing Suburb farmland replication 6 times respectively, Precision test result is as shown in table 1, and electric hot plate disappears to boil with the inventive method blank background value and sample recovery rate that boils that disappear and sees Table 2.
Table 1, Precision test result (n=6)
Table 2, electric hot plate disappear and boil sample blank background value and the sample recovery rate that disappears and boil with the inventive method
From Table 1 and Table 2, the inventive method accuracy and degree of accuracy are all better, and relative deviation and the recovery are all in the error range that allows.
Claims (4)
1. the assay method of arsenic content in the Plants is characterized in that: its testing process: the plant sample 0.5g after taking by weighing 100 orders and sieving, place 50mL band scale tool plug glass color comparison tube, and add red fuming nitric acid (RFNA) HNO
35mL adds a cover soaked overnight, does simultaneously the n.s. reagent blank; Disappear in 100 ℃ of water-baths and boil 2 hours next day, disappear boil end after, place Vapor Block to catch up with sour device, it is dried under 120 ℃ to 130 ℃ nitric acid to be evaporated to; After catching up with acid to finish, take off color comparison tube, cooling adds hydrochloric acid 5mL, 50g/L thiocarbamide+50g/L ascorbic acid mixed liquor 5mL, and ultrapure water is settled to 25mL, mixing, upper atomic fluorescence analysis instrument is measured arsenic content after filtering.
2. the assay method of arsenic content in the plant according to claim 1 is characterized in that: described disappearing boiled sample and directly placed Vapor Block to catch up with sour device to catch up with acid in the glass color comparison tube.
3. the assay method of arsenic content in the plant according to claim 1, it is characterized in that: described water-bath process is to place two row, six hole electric-heated thermostatic water baths.
4. the assay method of arsenic content in the plant according to claim 1 is characterized in that: Zeeman GFAAS: adopt the Hydrides AFS spectrometer analysis, reductive agent is 1% potassium borohydride+0.2% potassium hydroxide, and 5%HCL is as current-carrying.
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Cited By (7)
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| CN103499559A (en) * | 2013-10-15 | 2014-01-08 | 福建省邵武市永飞化工有限公司 | Method for measuring content of arsenic in fluorite powder |
| CN104502467A (en) * | 2014-11-20 | 2015-04-08 | 华中科技大学 | Determination method of arsenic valence |
| CN104677888A (en) * | 2015-03-06 | 2015-06-03 | 辽宁省分析科学研究院 | Method for measuring content of impurity elements in nuclear pump cleaning fluid |
| CN105466904A (en) * | 2014-08-22 | 2016-04-06 | 中国科学院生态环境研究中心 | Method for detection of arsenic in underground water |
| CN106053171A (en) * | 2016-05-27 | 2016-10-26 | 中粮集团有限公司 | Inorganic arsenic extraction method, method for determination of inorganic arsenic in rice and application of inorganic arsenic extraction method |
| CN106124467A (en) * | 2016-06-21 | 2016-11-16 | 何文 | A kind of soil activation state arsenic, bismuth, the detection method of antimony |
| CN110749583A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Detection method for measuring arsenic in soil and sediment by using atomic fluorescence |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103499559A (en) * | 2013-10-15 | 2014-01-08 | 福建省邵武市永飞化工有限公司 | Method for measuring content of arsenic in fluorite powder |
| CN105466904A (en) * | 2014-08-22 | 2016-04-06 | 中国科学院生态环境研究中心 | Method for detection of arsenic in underground water |
| CN104502467A (en) * | 2014-11-20 | 2015-04-08 | 华中科技大学 | Determination method of arsenic valence |
| CN104502467B (en) * | 2014-11-20 | 2016-08-31 | 华中科技大学 | A kind of assay method of arsenic valence state |
| CN104677888A (en) * | 2015-03-06 | 2015-06-03 | 辽宁省分析科学研究院 | Method for measuring content of impurity elements in nuclear pump cleaning fluid |
| CN106053171A (en) * | 2016-05-27 | 2016-10-26 | 中粮集团有限公司 | Inorganic arsenic extraction method, method for determination of inorganic arsenic in rice and application of inorganic arsenic extraction method |
| CN106124467A (en) * | 2016-06-21 | 2016-11-16 | 何文 | A kind of soil activation state arsenic, bismuth, the detection method of antimony |
| CN110749583A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Detection method for measuring arsenic in soil and sediment by using atomic fluorescence |
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Application publication date: 20130424 |