CN102879392A - Method for detecting uranium content of plant body - Google Patents
Method for detecting uranium content of plant body Download PDFInfo
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- CN102879392A CN102879392A CN2012103891672A CN201210389167A CN102879392A CN 102879392 A CN102879392 A CN 102879392A CN 2012103891672 A CN2012103891672 A CN 2012103891672A CN 201210389167 A CN201210389167 A CN 201210389167A CN 102879392 A CN102879392 A CN 102879392A
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Abstract
The invention discloses a method for detecting the uranium content of a plant body. The method is characterized by comprising the following steps of: washing, air-drying and weighing a plant picked up from a uranium-contaminated environment, performing drying, ashing and calcination treatment, and detecting the uranium content of the plant by using microtitration with the reduction of ammonium vanadate by titanous chloride. The method is applied to the detection of a plant sample with the uranium content of 0.003 to 0.03 percent, covers the whole range of the uranium content of all plant bodies to be detected collected in a uranium mine area, is short in detection time, clear in titration endpoint, accurate in result, convenient, low in cost, wide in application range and significant for researches on the environmental management of the uranium mine area, and has a good detection effect; the uranium content of the plant is rapidly detected by using a titration method; apparatuses required by the detection method are simple; the interference of other heavy metals in the plant body to a detection process is avoided; and a standard solution recovery experimental research result shows that a detection error is only 3/100,000.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to a kind of detection method of uranium content in the growing plants body that detects in the uranium contaminated environment, be specifically related to a kind of method that detects uranium content in the plant.
Background technology
Be grown in by the plant in the uranium contaminated environment throughout the year, adsorbed many kinds of metal ions in the soil, especially uranium ion by root system.To uranium content in the plant in the uranium contaminated environment carry out fast, make things convenient for, accurately, in batches detection, not only the rapid screening of uranium enriching plant in the uranium contaminated environment there is close relationship, simultaneously to the phytoremediation in the uranium contaminated environment, the energy-saving and emission-reduction research of the base material improvement in the restoration of the ecosystem of uranium ore Abandoned Land of Mine and the process of reconstruction, revegetation and Uranium there is very important meaning.But up to now, the detection methods such as ICP-AES, ICP-MS are generally adopted in the detection of uranium content in the plant, the defective such as that these methods exist is expensive, time-consuming, bothersome, effort.
Summary of the invention
The object of the present invention is to provide a kind of method that detects uranium content in the plant.
The present invention is achieved through the following technical solutions: will adopt next plant through after cleaning, dry, weighing from the uranium contaminated environment, again through oven dry, ashing, calcination processing is taken out and is cooled off to get sample; Again to sample pretreating: in the sample crucible, with hydrochloric acid and hydrogen peroxide it is processed, heating evaporation is to not bubbling, and phosphoric acid and hydrofluorite add thermal decomposition again, take off cooling after the decomposition, is used for washing beaker and residue with phosphoric acid,diluted, gets supernatant liquor after centrifugal;
Place beaker to adopt titanous reduction ammonium vanadate microtitrimetry to carry out titration supernatant liquor:
Drip l ferrous ammonium sulfate solution and enter in the beaker, and beaker is placed on the magnetic stirring apparatus, stir, drip again titanium trichloride, be purple to solution, after append again titanium trichloride; Drip afterwards the mixed solution of sodium nitrite and urea, shallow brownish black appears and after; Drip sodium hypobromite solution again, take off to brownish black, it is faint yellow that solution is; Drip again the mixed solution of described sodium nitrite and urea, behind the generation bubble, be stirred to bubble and eliminate, put clearly; Drip again the diphenylamine sulfonic acid sodium salt indicator, stir; Dripping the ammonium vanadate standard solution, to be titrated to little aubergine be terminal point again; Write down and consume ammonium vanadate standard solution volume, do simultaneously reagent blank and consume ammonium vanadate standard solution volume, detect the content of uranium in the plant by titanous reduction ammonium vanadate microtitrimetry.
Preferred concrete detection method is:
(1) pre-service of plant sample: sample cleaned weigh after drying, put into oven drying 3.5-4.5h of 100-110 ℃ to constant weight, with tissue mashing machine dried sample is smashed to pieces, weigh, the sample of smashing to pieces is placed on ashing on the flattening oven, put into 750-800 ℃ muffle furnace after the ashing and calcine 25-35min, take out and cool off to get sample;
(2) sample preparation: take by weighing 0.1-0.5g said sample in the 50ml crucible, it is wetting to add 0.5-1.5 ml waters, add 0.8-1.2ml concentration and be 37.5% hydrochloric acid and 0.4-0.6ml concentration and be 30% hydrogen peroxide heating evaporation to not bubbling, adding 2.5-3.5ml concentration again and be 85% phosphoric acid and 0.8-1.2ml concentration is 47% hydrofluorite, on 200 ℃ of-220 ℃ of control-temperature electric heating plates, add thermal decomposition 12-18min, take off cooling, sample solution is changed in the centrifuge tube, and be that 85% phosphoric acid mixes take volume ratio as 1:4 with water with concentration, mixed phosphoric acid liquid is used for the residue of washing crucible, solution also adds in the centrifuge tube in the lump after will washing, and with sample and sample cleansing solution cumulative volume constant volume at centrifuge tube 10ml place, shake up, centrifuge tube is put on the hydro-extractor, with the centrifugal 8-12min of 3600r/min rotating speed, take out centrifuge tube, supernatant liquor is poured in the 50ml glass beaker;
(3)Titanous reduction ammonium vanadate microtitrimetry: in the above-mentioned supernatant of pouring in the 50ml beaker, coming every of titration with dropper is 0.05ml, adding 2 concentration and be 10% l ferrous ammonium sulfate solution enters in the beaker, and beaker placed on the magnetic stirring apparatus, put into stirrer, start power supply and stir, drip again concentration and be 15% titanium trichloride, be purple to solution, append again 1 concentration and be 15% titanium trichloride; Drip again afterwards 5% sodium nitrite and 15% urea according to the mixed solution of volume ratio 1:1, after shallow brownish black occurring, dripping concentration is the sodium hypobromite solution of 0.3mol/L again, take off to brownish black, it is faint yellow that solution is, drip again 10 described urea-sodium nitrite mixed liquors, produce bubble, stir 0.8-2min, bubble eliminates, powered-down is placed 1-2min, adds 2-4 diphenylamine sulfonic acid sodium salt indicator, starting power supply stirs, open microburette, being titrated to little aubergine with the ammonium vanadate standard solution is terminal point again, writes down to consume ammonium vanadate standard solution volume; Do simultaneously reagent blank and consume ammonium vanadate standard solution volume, be calculated as follows analysis result:
T-ammonium vanadate standard solution is to the titer g/ml of uranium;
V-titration consumes ammonium vanadate standard solution volume ml;
V0-titration reagent blank consumes ammonium vanadate standard solution volume ml;
M-title sample quality g;
Above-described number percent is mass percent if no special instructions.
The present invention is applicable to the detection of uranium-bearing 0.003% ~ 0.03% plant sample, contain uranium content scope in all plants to be detected that the uranium ore mining area collects, use titrimetry that uranium content in the plant is carried out fast detecting, the required instrument of detection method is simple, detection time is short, detect effective, the result is accurate, method is easy, and cost is low, and the utilization scope is wide, testing process is not subjected to the interference of other heavy metals in the plant, show that by standard solution recovery test result of study error only differs 3/100000ths, the research that the uranium ore area surroundings is administered has great significance.
Embodiment
The present invention is by following example can the invention will be further described, yet scope of the present invention is not limited to following example.
Embodiment 1:
With the uranium ore beggar-ticks (
BidenspilosaLinn.) be example, detailed experimental implementation process is as follows:
(1) beggar-ticks pre-service
Beggar-ticks being connected (contain root, stem, leaf, flower, really) gathers, clean dry after, put into 105 ℃ oven drying 4h to constant weight, with tissue mashing machine dried sample is smashed to pieces, (m weighs
1: 25.309g), the sample of smashing to pieces is placed on ashing and the (m that weighs on the flattening oven
2: 3.216g), take by weighing sample (m after the ashing
3: 2.849g), put into 750 ℃ muffle furnace and calcine 30min, take out and cool off to get sample and the (m that weighs
4: 1.833g).
Take by weighing pretreated sample (m
5: 0.489g) in the 50ml crucible, the material of crucible is teflon, add the 1ml water-wet, add 1ml concentration and be the hydrogen peroxide heating evaporation of 37.5% hydrochloric acid and 0.5ml 30% to not bubbling, add again 3ml85% phosphoric acid and 1ml47% hydrofluorite, on 200 ℃ of control-temperature electric heating plates, add thermal decomposition 15min, take off cooling, sample solution is changed in the centrifuge tube, and be that 85% phosphoric acid mixes take volume ratio as 1:4 with water with concentration, mixed phosphoric acid liquid is used for the residue of washing crucible, and will wash afterwards, solution also adds in the centrifuge tube in the lump, and with sample and sample cleansing solution cumulative volume constant volume at centrifuge tube 10ml place, shake up, centrifuge tube is put on the hydro-extractor, with the centrifugal 10min of 3600r/min rotating speed, take out centrifuge tube, supernatant liquor is poured in the 50ml glass beaker.
(2) titration testing process
In the above-mentioned supernatant of pouring in the 50ml beaker, coming every of titration with dropper is 0.05ml, drip 2 10% l ferrous ammonium sulfate solution, place on the magnetic stirring apparatus, put into stirrer, start power supply and stir, drip 2-3 and drip 15% titanium trichloride, be purple to solution, solution is that to append 1 concentration behind the purple be 15% titanium trichloride again; Drip again afterwards 5% sodium nitrite and 15% urea according to the mixed solution of volume ratio 1:1, shallow brownish black appears, add again 7 ~ 8 0.3mol/L sodium hypobromite solution, take off to brownish black, it is faint yellow that solution is, and drips 10 described urea-sodium nitrite mixed liquors again, produce bubble, stir 1min, bubble eliminates, powered-down, place 1 ~ 2min, add 2 ~ 4 diphenylamine sulfonic acid sodium salt indicator, start power supply and stir, open again microburette, during the microburette titration, every is 0.02ml, and being titrated to little aubergine with the ammonium vanadate standard solution is terminal point, writes down to consume ammonium vanadate standard solution volume V(V=4.767ml); Do simultaneously reagent blank and consume ammonium vanadate standard solution volume V
0(V
0=0.02ml).
(2) beggar-ticks adsorption uranium cubage process
Uranium content in the sample after the calcining
ω 1, (wherein ammonium vanadate titer is
T U / NH4VO3 =0.1389
Mg/ml )
Plant adsorption uranium content
ω
Wherein:
T is the titer of ammonium vanadate,
Mg/ml
V is the volume that titration consumes Ammonium Vanadate Solution, ml;
V
0For the blank volume that consumes Ammonium Vanadate Solution of titration is 0.02ml;
m
1Be plant dry weight before the carbonization, g;
m
2Be grey weight after the carbonization, g;
m
3Be that plant ass is heavy before 750 ℃ of calcinings, g;
m
4Heavy for calcining rear plant ass, g;
Above-described number percent is mass percent if no special instructions.
Calculate by formula, obtaining at last beggar-ticks adsorption uranium content is 0.110mg/g.
Claims (3)
1. method that detects plant adsorption uranium content is characterized in that: will adopt the plant that comes through after cleaning, dry, weighing from the uranium contaminated environment, again through oven dry, ashing, calcination processing is taken out and is cooled off to get sample; Again to sample pretreating: in the sample crucible, with hydrochloric acid and hydrogen peroxide it is processed, heating evaporation is to not bubbling, and phosphoric acid and hydrofluorite add thermal decomposition again, take off cooling after the decomposition, is used for washing beaker and residue with phosphoric acid,diluted, gets supernatant liquor after centrifugal;
Place beaker to adopt titanous reduction ammonium vanadate microtitrimetry to carry out titration supernatant liquor:
Drip l ferrous ammonium sulfate solution and enter in the beaker, and beaker is placed on the magnetic stirring apparatus, stir, drip again titanium trichloride, be purple to solution, after append again titanium trichloride one time; Drip afterwards the mixed solution of sodium nitrite and urea, shallow brownish black appears and after; Drip sodium hypobromite solution again, take off to brownish black, it is faint yellow that solution is; Drip again the mixed solution of described sodium nitrite and urea, behind the generation bubble, be stirred to bubble and eliminate, put clearly; Drip again the diphenylamine sulfonic acid sodium salt indicator, stir; Dripping the ammonium vanadate standard solution, to be titrated to little aubergine be terminal point again; Write down and consume ammonium vanadate standard solution volume, do simultaneously reagent blank and consume ammonium vanadate standard solution volume, detect the content of uranium in the plant by titanous reduction ammonium vanadate microtitrimetry.
2. as weighing a kind of method that detects uranium content in the plant as described in 1, it is characterized in that operation steps and testing process are followed successively by:
(1) pre-service of plant sample: sample cleaned weigh after drying, put into oven drying 3.5-4.5h of 100-110 ℃ to constant weight, with tissue mashing machine dried sample is smashed to pieces, weigh, the sample of smashing to pieces is placed on ashing on the flattening oven, put into 750-800 ℃ muffle furnace after the ashing and calcine 25-35min, take out and cool off to get sample;
(2) sample preparation: take by weighing 0.1-0.5g said sample in the 50ml crucible, it is wetting to add 0.5-1.5 ml waters, add 0.8-1.2ml concentration and be 37.5% hydrochloric acid and 0.4-0.6ml concentration and be 30% hydrogen peroxide heating evaporation to not bubbling, adding 2.5-3.5ml concentration again and be 85% phosphoric acid and 0.8-1.2ml concentration is 47% hydrofluorite, on 200 ℃ of-220 ℃ of control-temperature electric heating plates, add thermal decomposition 12-18min, take off cooling, sample solution is changed in the centrifuge tube, and be that 85% phosphoric acid mixes take volume ratio as 1:4 with water with concentration, mixed phosphoric acid liquid is used for the residue of washing crucible, solution also adds in the centrifuge tube in the lump after will washing, and with sample and sample cleansing solution cumulative volume constant volume at centrifuge tube 10ml place, shake up, centrifuge tube is put on the hydro-extractor, with the centrifugal 8-12min of 3600r/min rotating speed, take out centrifuge tube, supernatant liquor is poured in the 50ml glass beaker;
(3)Titanous reduction ammonium vanadate microtitrimetry: in the above-mentioned supernatant of pouring in the 50ml beaker, coming every of titration with dropper is 0.05ml, adding 2 concentration and be 10% l ferrous ammonium sulfate solution enters in the beaker, and beaker placed on the magnetic stirring apparatus, put into stirrer, start power supply and stir, drip again concentration and be 15% titanium trichloride, be purple to solution, append again 1 concentration and be 15% titanium trichloride; Drip again afterwards 5% sodium nitrite and 15% urea according to the mixed solution of volume ratio 1:1, after shallow brownish black occurring, dripping concentration is the sodium hypobromite solution of 0.3mol/L again, take off to brownish black, it is faint yellow that solution is, drip again 10 described urea-sodium nitrite mixed liquors, produce bubble, stir 0.8-2min, bubble eliminates, powered-down is placed 1-2min, adds 2-4 diphenylamine sulfonic acid sodium salt indicator, starting power supply stirs, open microburette, being titrated to little aubergine with the ammonium vanadate standard solution is terminal point again, writes down to consume ammonium vanadate standard solution volume; Do simultaneously reagent blank and consume ammonium vanadate standard solution volume, be calculated as follows analysis result:
T-ammonium vanadate standard solution is to the titer g/ml of uranium;
V-titration consumes ammonium vanadate standard solution volume ml;
V0-titration reagent blank consumes ammonium vanadate standard solution volume ml;
M-title sample quality g;
Above-described number percent is mass percent if no special instructions.
3. as weighing a kind of method that detects uranium content in the plant as described in 2, the material that it is characterized in that crucible is teflon.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104359751A (en) * | 2014-12-01 | 2015-02-18 | 核工业理化工程研究院 | Method for determining trace uranium in soil by microwave digestion fluorescence method |
| CN106018713A (en) * | 2016-05-03 | 2016-10-12 | 成都亿信标准认证集团有限公司 | Automatic food heavy metal detecting system |
| CN106595794A (en) * | 2016-12-31 | 2017-04-26 | 从俊强 | Iron-containing powder true volume detecting method based on constant volume method |
| CN109211630A (en) * | 2018-09-14 | 2019-01-15 | 徐州工程学院 | A kind of rapid detection method of content of heavy metal in foods |
| CN109541126A (en) * | 2018-12-19 | 2019-03-29 | 中核北方核燃料元件有限公司 | The measuring method of uranium content in a kind of U-Mo Alloy |
| CN110412642A (en) * | 2019-07-19 | 2019-11-05 | 湖北兴福电子材料有限公司 | The detection method of total α particle in a kind of phosphoric acid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104359751A (en) * | 2014-12-01 | 2015-02-18 | 核工业理化工程研究院 | Method for determining trace uranium in soil by microwave digestion fluorescence method |
| CN106018713A (en) * | 2016-05-03 | 2016-10-12 | 成都亿信标准认证集团有限公司 | Automatic food heavy metal detecting system |
| CN106595794A (en) * | 2016-12-31 | 2017-04-26 | 从俊强 | Iron-containing powder true volume detecting method based on constant volume method |
| CN109211630A (en) * | 2018-09-14 | 2019-01-15 | 徐州工程学院 | A kind of rapid detection method of content of heavy metal in foods |
| CN109541126A (en) * | 2018-12-19 | 2019-03-29 | 中核北方核燃料元件有限公司 | The measuring method of uranium content in a kind of U-Mo Alloy |
| CN110412642A (en) * | 2019-07-19 | 2019-11-05 | 湖北兴福电子材料有限公司 | The detection method of total α particle in a kind of phosphoric acid |
| CN110412642B (en) * | 2019-07-19 | 2022-12-16 | 湖北兴福电子材料有限公司 | Method for detecting total alpha particles in phosphoric acid |
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Application publication date: 20130116 |