CN102288585A - Method for measuring trace uranium (VI) element by specific fluorescent reagent - Google Patents
Method for measuring trace uranium (VI) element by specific fluorescent reagent Download PDFInfo
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- CN102288585A CN102288585A CN2011101143780A CN201110114378A CN102288585A CN 102288585 A CN102288585 A CN 102288585A CN 2011101143780 A CN2011101143780 A CN 2011101143780A CN 201110114378 A CN201110114378 A CN 201110114378A CN 102288585 A CN102288585 A CN 102288585A
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- uranium
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- AAORDHMTTHGXCV-UHFFFAOYSA-N uranium(6+) Chemical compound [U+6] AAORDHMTTHGXCV-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 7
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 24
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 23
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 22
- 230000005284 excitation Effects 0.000 claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 238000012921 fluorescence analysis Methods 0.000 claims abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 4
- COQLPRJCUIATTQ-UHFFFAOYSA-N Uranyl acetate Chemical compound O.O.O=[U]=O.CC(O)=O.CC(O)=O COQLPRJCUIATTQ-UHFFFAOYSA-N 0.000 abstract 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 21
- 239000000243 solution Substances 0.000 description 20
- 229910052770 Uranium Inorganic materials 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 9
- 238000007865 diluting Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- ABUBSBSOTTXVPV-UHFFFAOYSA-H [U+6].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O Chemical compound [U+6].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O ABUBSBSOTTXVPV-UHFFFAOYSA-H 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 239000012472 biological sample Substances 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 ore Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 125000005289 uranyl group Chemical group 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明公开了一种特效荧光试剂测定微量铀(VI)元素的方法，荧光分析的条件为：在硝酸介质中，在pH为4.0时，苯甲酸和罗丹明B摩尔比为1∶1的条件下，铀(VI)能与苯甲酸和罗丹明B形成稳定的配位化合物；所述铀(VI)的配合物的最佳激发波长为260nm，发射波长为575nm，激发和发射狭缝为：5.0nm和3.0nm。用醋酸双氧铀溶液作样品检测，实验值与理论值相符，该方法准确可靠。
The invention discloses a method for measuring trace uranium (VI) elements with a special-effect fluorescent reagent. The condition of the fluorescence analysis is: in a nitric acid medium, when the pH is 4.0, the molar ratio of benzoic acid and rhodamine B is 1:1. Under this condition, uranium (VI) can form a stable coordination compound with benzoic acid and rhodamine B; the optimum excitation wavelength of the complex of the uranium (VI) is 260nm, and the emission wavelength is 575nm, and the excitation and emission slits are: 5.0nm and 3.0nm. Uranyl acetate solution was used as sample detection, the experimental value was consistent with the theoretical value, the method is accurate and reliable.
Description
Technical field
The present invention relates to a kind of special efficacy fluorescent reagent and measure the method for trace uranium (VI) element, belong to chemical analysis field.
Background technology
Uranium is present in the materials such as industrial waste water, ore, cinder, rare earth material, glass and pottery.In standard GB/T11848.1-2008 uranium ore concentrate analytical approach, the GB11223.1-1989 biological sample ash in the mensuration solid fluorimetry of uranium, the GB6768-86 water trace uranium analytical approach be difficult to buy corresponding fluorescence-enhancing agent, the mensuration of uranium generally adopts uranol-III or 5-Br-PADAP photometry, the swollen III method of azo, to ethoxy dibromo arsenazo method etc., but condition determination is restive.
Summary of the invention
Technical matters to be solved by this invention is at the deficiencies in the prior art, provides a kind of special efficacy fluorescent reagent of being convenient to operate, conveniently control to measure the method for trace uranium (VI) element, adopts following technical scheme:
A kind of special efficacy fluorescent reagent is measured the method for trace uranium (VI) element, the condition of fluorescence analysis is: in nitric acid medium, at pH is 4.0 o'clock, and benzoic acid and rhodamine B mol ratio are that uranium (VI) can form stable coordination compound with benzoic acid and rhodamine B under 1: 1 the condition; The maximum excitation wavelength of the complex of described uranium (VI) is 260nm, and emission wavelength is 575nm, excites and launch slit to be: 5.0nm and 3.0nm.
Make sample detection with uranium acetate solution, experiment value conforms to theoretical value, and this method accurately and reliably.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of three kinds of different excitation wavelengths; (1,260nm; 2,240nm; 3,270nm; 4,310nm);
Fig. 2 excites the fluorescence spectrum figure of slit and emission slit for 260nm excites difference; (1, excite slit 2.5, emission slit 3.0; 2, excite slit 2.5, emission slit 2.5; 3, excite slit 5.0, emission slit 3.0; 4, excite slit 6.0, emission slit 3.0);
Fig. 3 is the typical curve of uranium.
Embodiment
The present invention selects benzoic acid and rhodamine B to make the developer of uranium (VI), studies the chromogenic reaction of itself and uranium (VI), inquires into the top condition of reaction, records the content of trace uranium (VI), obtains better effects.Reaction mechanism is as follows:
1.1 key instrument and equipment
The key instrument, the equipment that use in the test are as shown in table 1.
Table 1 test key instrument and equipment
| The instrument title | Model | Manufacturer |
| Fluorospectrophotometer | ?LS55 | U.S. PE company |
| Acidometer | ?DOS-11A | Chengdu Noah's ark scientific and technological development company |
| Electronic balance | ?FA604A | The triumphant grand company limited already in Beijing |
| The ultrasonic cleaning instrument | ?KQ2200E | Kunshan Ultrasonic Instruments Co., Ltd. |
1.2 main agents
Medicine used in the present invention sees table 2 for details.
Table 2 main agents
| Nomenclature of drug | Type | Manufacturer | Chemical formula |
| Uranyl nitrate | Analyze pure | Made in China | ?UO2(NO3)2·6H2O |
| Uranium acetate | Analyze pure | Made in China | ?UO2(CH3CO2)·2H2O |
| Benzoic acid | Analyze pure | Dragon chemical industry examination factory of Chengdu section | ?C7H6O2 |
| Rhodamine B | Analyze pure | Close sour manufacturing plant of Tianjin section | ?C28H31CLN2O3 |
| NaOH | Analyze pure | Dragon chemical industry examination factory of Chengdu section | ?NaOH |
| Nitric acid | Analyze pure | Dragon chemical industry examination factory of Chengdu section | ?HNO3 |
1.3 experimental procedure
1.3.1 experimental solutions preparation
1. the preparation of uranyl nitrate
Accurately take by weighing the uranyl nitrate of 50.133mg with 1,000,000/balance (0.001mg), pour in the 50mL beaker of cleaning in advance, add about 20mL distilled water, solution is moved in the volumetric flask of 100mL, and with distilled water diluting to scale, be mixed with 0.9982 * 10
-4MolL
-1Preserve.
2. the preparation of uranium acetate solution
Accurately take by weighing the uranium acetate of 46.507mg with 1,000,000/balance (0.001mg), pour in the 50mL beaker of cleaning in advance, add about 20mL distilled water, solution is moved in the volumetric flask of 100mL, and with distilled water diluting to scale, 1.0964 * 10
-4MolL
-1Preserve.
3. the preparation of benzoic acid solution
Accurately take by weighing the benzoic acid of 12.669mg with 1,000,000/balance (0.001mg), pour in the 50mL beaker of cleaning in advance, add about 20mL distilled water, solution is moved in the volumetric flask of 100mL, and with distilled water diluting to scale, 1.011 * 10
-4MolL
-1Preserve.
4. the preparation of rhodamine B solution
Accurately take by weighing the rhodamine B of 45.101mg with 1,000,000/balance (0.001mg), pour in the 50mL beaker of cleaning in advance, add about 20mL distilled water, solution is moved in the volumetric flask of 100mL, and with distilled water diluting to scale, 0.9415 * 10
-4MolL
-1Preserve.
5. acid-base solution preparation (adjusting pH value)
(1) NaOH: accurately take by weighing 4.0g NaOH, pour clean beaker into, add the suitable quantity of water dilution, the solution after will diluting again joins in the volumetric flask of 100mL, adds water to scale, shakes up to get final product.Concentration is molL-1.Waiting needs the time spent, is diluted to desired concn.
(2) nitric acid: accurately take by weighing the red fuming nitric acid (RFNA) of 9.69g65%, pour clean beaker into, add the suitable quantity of water dilution, the solution after will diluting again joins in the volumetric flask of 100mL, adds water to scale, shakes up to get final product.Concentration is molL-1.Waiting needs the time spent, is diluted to desired concn.
1.3.2 the selection of developer
1. the complex of uranium is selected
At excitation wavelength 310nm, emission wavelength 596nm excites slit 5.0 to uranyl nitrate, benzoic acid solution, rhodamine B solution, and the emission slit is measured fluorescence intensity 3.0 times, obtains the results are shown in Table 3.As can be seen from Table 3: the uranium individualism does not have fluorescence, and mixing with benzoic acid does not have fluorescence yet.Uranyl nitrate has stronger fluorescence after the mixing of benzoic acid and rhodamine B.
The Different Complex fluorescence intensity table of table 3 uranium
The fluorescence intensity of table 4 different mixture ratio
2. benzoic acid and rhodamine B match ratio are selected
At excitation wave 310nm, transmitted wave 596nm excites slit 5.0, and emission slit 3.0 times benzoic acid and rhodamine B measured in solution fluorescence intensities to different proportionings obtain result such as table 4.Can draw by last table 4 result: benzoic acid and rhodamine B the two than being that 1: 1 o'clock fluorescence is the strongest.
1.3.3 the best excites the selection with emission wavelength and slit
1. the best selection that excites with emission wavelength
With uranium and benzoic acid and rhodamine B three ratio is that 1: 1: 1 mixed liquor is made Fig. 1, and as can be seen from Figure 1 at exciting light during at the 260nm place, resulting exciting light spectrogram intensity is moderate, and is disturbed lessly, and intensity is bigger.Between 550nm-610nm, promptly there is big emission wavelength at the 575nm place.
2. the selection of slit
With uranium and benzoic acid and rhodamine B three mol ratio is 1: 1: 1 mixed liquor, with the optical excitation of 260nm, selects difference to excite and launches slit and do the fluorescence spectrum mapping, as shown in Figure 2.As seen exciting slit from Fig. 2: 5.0nm, the emission slit: 3.0 exciting light spectrogram intensity are moderate, and disturbed lessly, and the peak type is level and smooth, herein best results.
1.3.4 system acidity is selected
1: 1 mixed liquor of benzoic acid and rhodamine B is at excitation wave 260nm, and transmitted wave 575nm excites slit 5.0, and the emission slit is measured different pH fluorescence intensities for 3.0 times, obtains result such as table 5.As can be seen from Table 5, adopt nitric acid as medium, mixed liquor is the fluorescence intensity maximum when pH=4.
The different pH values of table 5 are the fluorescence intensity of mixed liquor down
| PH | Mixed liquor (1: 1) |
| 2.0 | 159.723 |
| 4.0 | 184.699 |
| 6.0 | 184.026 |
| 8.0 | 160.220 |
1.3.5 the influence of coexisting ion
The fluorescence intensity that table 6 different ions is disturbed
| Ion | ?Na + | K + | Ca 2+ | Pb 2+ | Ni 2+ | Cu 2+ | Mg 2+ | Al 3+ | Co 2+ | Hg + | Ag + | Fe 3+ | NO 3 |
| Intensity (int) | ?86 | 144 | 182 | 183 | 187 | 180 | 190 | 187 | 175 | 185 | 186 | 56 | 183 |
Can find out that from table 6 add common interfering ion in the mixed liquor that uranium (VI) exists, the result shows Ca
2+, Pb
2+, Ni
2+, Zn
2+, Mg
2+, Al
3+, Co
2+, Hg
+, Ag
+, NO
3 -Deng very little to its fluorescence influence in the milligram level.Na
+, K
+Uranium solution there is the effect of weakening.Fe
3+Interference effect is also arranged, but Fe
3+Allowance can reach 100 times, can add EDTA and shelter, can eliminate interference.
1.3.6 stability test
Compound concentration is 2.4 * 10
-7The uranium of mol/L (VI) solution is used excitation wave 260nm, and transmitted wave 575nm excites slit 5.0, and the emission slit is measured the different time fluorescence intensity 3.0 times, sees Table 7.
Fluorescence intensity under table 7 different time
| Time (min) | 5 | 10 | 20 | 30 | 60 |
| Intensity (int) | 254.14 | 253.80 | 254.70 | 254.65 | 253.64 |
As shown in Table 7, the intensity of solution is little with the variation of sweep time, and the complex of uranium (VI) is more stable.
1.3.7 lowest detection line
According to above-mentioned test condition.Original mixed liquid is diluted to 250 times respectively, 500 times, 1000 times, 2000 times, 5000 times, 10000 times.Uranium (VI) solution concentration is respectively 3.992 * 10
-7MolL
-1, 1.996 * 10
-7MolL
-1, 0.9982 * 10
-7MolL
-1, 0.4991 * 10
-7MolL
-1, 0.1996 * 10
-7MolL
-1, 0.9982 * 10
-8MolL
-1Record fluorescence intensity and see Table 8.
Table 8 dilution variable concentrations fluorescence intensity
| Extension rate | 250 times | 500 times | 1000 times | 2000 times | 5000 times | 10000 times |
| Fluorescence intensity | 355.51 | 196.5 | 106.71 | 55.24 | 21.28 | ?8.68 |
As can be seen from Table 8, the concentration of uranium (VI) detection lower limit is about 0.9982 * 10
-8MolL
-1
1.3.8 the drafting of typical curve
Get 6 10mL volumetric flasks, number 0-5 respectively.Get distilled water as blank solution, numbering 0.It is 1.996 * 10 that 1-5 adds concentration respectively
-7MolL
-1, 1.502 * 10
-7MolL
-1, 0.9982 * 10
-7MolL
-1, 0.4991 * 10
-7MolL
-1, 0.1996 * 10
-7MolL
-1The uranium mixed liquor, regulate pH=4, use excitation wavelength 260nm, emission wavelength 575nm excites slit 5.0nm, emission slit 3.0nm is mensuration down.Table sees 9 as a result.
The tabulation of table 9 typical curve
| Numbering | Concentration (mol/L10 -7) | Intensity | Background value |
| 0 | 0 | 0.117 | 8.584 |
| 1 | 0.2 | 21.252 | 8.584 |
| 2 | 0.5 | 55.540 | 8.584 |
| 3 | 1.0 | 106.718 | 8.584 |
| 4 | 1.5 | 147.289 | 8.584 |
| 5 | 2.0 | 196.547 | 8.584 |
Make Fig. 3 by table 9; Linear equation is y=-4.505x
2+ 105.424x+0.0 degree of fitting is: 0.9988
1.3.9 the mensuration of sample
Adopt the pure uranium acetate of analysis to measure as sample.Uranium acetate concentration is formulated as: 2.1928 * 10
-7MolL
-1, 1.0964 * 10
-7MolL
-1, 0.5482 * 10
-7MolL
-1(add 1: 1 benzoic acid of equivalent and rhodamine B mixed liquor, and regulate pH=4), use excitation wave 260nm, transmitted wave 575nm excites slit 5.0nm, and emission slit 3.0nm is mensuration down, sees Table 10.
The tabulation of table 10 sample determination
The result who records as shown in Table 10 conforms to substantially with normative reference, and relative error is 3.6%.
2 conclusions
The solution of uranium (VI) does not have fluorescence, but behind the complex that forms with specical regent benzoic acid and rhodamine B hyperfluorescence is arranged, and can measure the content of uranium (VI) element with the fluorescent liquid method.Be that uranium (VI) can form stable coordination compound with benzoic acid and rhodamine B under 1: 1 the condition in benzoic acid and rhodamine B mol ratio.In nitric acid medium, be 4.0 o'clock to be the optimum acidity that complex fluorescent is analyzed at pH.The maximum excitation wavelength of the complex of uranium (VI) is 260nm, and emission wavelength is 575nm, excites and launch slit to be: 5.0nm and 3.0nm.
Should be understood that, for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207153A (en) * | 2013-03-11 | 2013-07-17 | 中国原子能科学研究院 | Precise determination method for small amount of uranium |
| CN103592266A (en) * | 2012-08-14 | 2014-02-19 | 中国辐射防护研究院 | Method for quantitatively measuring infinitesimal amount of uranium in steel |
| CN103852455A (en) * | 2013-07-11 | 2014-06-11 | 北京安生绿源科技有限公司 | Equipment and method for quantitatively and rapidly detecting uranium at constant temperature in real time |
| CN105675554A (en) * | 2015-12-30 | 2016-06-15 | 谱尼测试科技(天津)有限公司 | Fluoro-spectrophotometry method for detecting total flavones in health-caring foods |
| CN105810278A (en) * | 2016-05-23 | 2016-07-27 | 绍兴文理学院 | Purification detection and purification device of uranium-polluted underground water |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103592266A (en) * | 2012-08-14 | 2014-02-19 | 中国辐射防护研究院 | Method for quantitatively measuring infinitesimal amount of uranium in steel |
| CN103207153A (en) * | 2013-03-11 | 2013-07-17 | 中国原子能科学研究院 | Precise determination method for small amount of uranium |
| CN103852455A (en) * | 2013-07-11 | 2014-06-11 | 北京安生绿源科技有限公司 | Equipment and method for quantitatively and rapidly detecting uranium at constant temperature in real time |
| CN103852455B (en) * | 2013-07-11 | 2017-04-12 | 北京安生绿源科技有限公司 | Equipment and method for quantitatively and rapidly detecting uranium at constant temperature in real time |
| CN105675554A (en) * | 2015-12-30 | 2016-06-15 | 谱尼测试科技(天津)有限公司 | Fluoro-spectrophotometry method for detecting total flavones in health-caring foods |
| CN105810278A (en) * | 2016-05-23 | 2016-07-27 | 绍兴文理学院 | Purification detection and purification device of uranium-polluted underground water |
| CN105810278B (en) * | 2016-05-23 | 2018-05-29 | 绍兴文理学院 | A kind of purification detection purifier of uranium polluted underground water |
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Application publication date: 20111221 |