CN106770118A - The assay method of arsenic content in a kind of water - Google Patents
The assay method of arsenic content in a kind of water Download PDFInfo
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- CN106770118A CN106770118A CN201611237805.3A CN201611237805A CN106770118A CN 106770118 A CN106770118 A CN 106770118A CN 201611237805 A CN201611237805 A CN 201611237805A CN 106770118 A CN106770118 A CN 106770118A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a kind of assay method of arsenic content in water, using total arsenic content in the type dual channel atomic fluorescence photometers of AFS 820 measure water, including：Sample solution is prepared, arsenic standard solution is prepared, sample solution is introduced into atomic fluorescence spectrophotometer, the fluorescence intensity of arsenic in determination sample solution, the fluorescence intensity that the arsenic standard solution according to concentration known is measured obtains the content of arsenic in sample solution.The method of the invention is improved based on GB GB/T 5,750 2006, and the method after improvement is simple to operate quick, with cost-effective, the advantages of data are reliable, and the more conducively practical operation of laboratory staff.
Description
Technical field
The invention belongs to monitoring water environment method field, and in particular to the assay method of arsenic content in a kind of water.
Background technology
Arsenic is widely present in nature, and is easy to be accumulated in human body, not only results in the acute and chronic poisoning of human body,
And also carcinogenesis, cutaneum carcinoma etc. can be caused.Therefore, preventing and controlling of the people to arsenic pollution are increasingly paid close attention to.In water ring
In the monitoring of border, arsenic has been listed in one of routine monitoring project.What the assay method of arsenic was commonly used has diethyldithiocar bamic acid
The new silver salt AAS of silver-colored AAS, zinc-sulfate system, arsenic spot method, catalytic polarographic method and inductive etc. from
Daughter mass spectrography（ICP-MS）Deng.
Because the sensitivity having is relatively low in the above method, some operating process are cumbersome, the reagent toxicity for being used having
Larger, some instruments are expensive, the factors such as high expensive is limited their use.Hydride generation-atomic fluorescence spectrometry light
Spectrometry is in radiation energy to excite the fluorescent emission intensity of lower generation by measuring the atomic vapour of element to be measured to determine unit to be measured
The method of cellulose content, have the advantages that sensitivity it is high, interference less, it is easy to operate quick, Biosample and environmental sample are divided
Analysis determines the effect that can have obtained.However, when using total arsenic content in GB GB/T 5750-2006 measure water recently, arsenic mark
The liquid rate of recovery is higher always, and what is had is up to more than 170% unexpectedly, and error is too big, makes measurement result inaccurate.
The content of the invention
It is an object of the invention to overcome above mentioned problem, there is provided the measure side of arsenic content in a kind of water for reducing error
Method.
To achieve the above object, the technical solution adopted in the present invention is specific as follows：
The assay method of arsenic content, comprises the following steps in a kind of water：
（1）Sample solution is prepared, process for preparation is：Water sample, reducing agent, pure hydrochloric acid are mixed, mixed solution is obtained, then
Mixed solution heating is carried out into digestion process, digestion records surplus solution volume, shakes up after terminating, and obtains sample solution, while
Do blank test；The reducing agent for thiourea and ascorbic acid mixed solution, and in mixed solution thiocarbamide and ascorbic acid matter
Amount concentration is 2.5%；
（2）Prepare arsenic standard solution；
（3）Sample solution is introduced into atomic fluorescence spectrophotometer, the fluorescence intensity of arsenic in determination sample solution, according to concentration known
The fluorescence intensity that arsenic standard solution is measured calculates the content of arsenic in sample solution.
Preferably, step（1）Middle water sample, reducing agent, pure hydrochloric acid are with 10:1:1 volume ratio is mixed.
Preferably, step（1）The condition of middle hot digestion treatment is：Mixed solution places 40 under 100 DEG C of water-baths
min。
Preferably, step（1）Described in the compound method of thiourea and ascorbic acid mixed solution be：Weigh 2.5 g thiocarbamides and
2.5 g ascorbic acid are dissolved in 100 mL ultra-pure waters, are shaken up standby.
Preferably, step（1）It is middle prepare sample solution when detailed process be：The mL of water sampling 10, adds 1.0 mL reduction
Agent, adds 1.0 mL pure hydrochloric acids, is well mixed, and 40 min are placed under 100 DEG C of water-baths, records surplus solution volume, shakes up
Sample solution.
The preparation of the main agents used in this experimentation：
Arsenic standard reserving solution：GBW(E)080215（China National Measuring Science Research Inst. produces）, the concentration of this standard reserving solution is 100
ug/mL（Specific compound method is with described in GB GB/T 5750-2006）；
Arsenic standard working solution：As required, the ug/mL standard working solutions containing arsenic 0.1 are prepared with above-mentioned arsenic standard reserving solution, is stored in
It is standby in polyethylene bottle；
Thiourea and ascorbic acid mixed solution：Weigh 2.5 g thiocarbamides and 2.5 g ascorbic acid are dissolved in 100 mL ultra-pure waters, shake up
It is standby；
Potassium borohydride and potassium hydroxide solution：20 g potassium borohydrides and 5 g potassium hydroxide are weighed, 1000 mL distilled water are added to
In, shaking up makes to be completely dissolved, and is stored in standby in polyethylene bottle；
Hydrochloric acid：Measure 25 mL pure hydrochloric acids（Ultra-clean extra pure regent）, be slowly added into the distilled water of 400 mL or so, and with steam
Distilled water is diluted to 500 mL.
The beneficial effects of the invention are as follows：
Arsenic content in assay method of the invention and People's Republic of China's standard GB/T 5750.6-2006 Drinking Waters
The general principle of assay method is consistent, is with the sulphur of low concentration when simply in assay method of the invention prepared by sample solution
Urea and ascorbic acid mixed solution.To the consumption of reducing agent that is constituted with acid amount, thiocarbamide and ascorbic acid in experimentation and
The links such as its standing time find after being checked, although the thiocarbamide and ascorbic acid solution in GB using higher concentration can rise
Shielded and reduction to more preferable, but the degree of accuracy of Instrument measuring can be influenceed, make measurement result higher, and use low concentration
Thiocarbamide and ascorbic acid mixed liquor can reduce the error occurred in continuous mode, make measurement result more accurate.Use state simultaneously
Family's arsenic standard solution can directly prepare standard curve, and easy to operate, accuracy is high, and linear relationship is good.In sum, present invention side
Method has the advantages that to operate flexible, cost-effective, data reliable, is more beneficial for the practical operation of laboratory staff.
Specific embodiment
With reference to specific embodiment, technical solution of the present invention is described in further detail.
Embodiment, the assay method of arsenic content in a kind of water
1.1 general principles
In acid condition, trivalent arsenic and potassium borohydride reaction generation arsenic hydride, by carrier gas（Argon gas）Bring quartz atomizer into,
It is heated and is decomposed into atomic state arsenic.Under the irradiation of special as hollow cathode lamp, ground state arsenic atom is excited to upper state, in deactivation
When change returns to ground state, launch the fluorescence of characteristic wavelength, in the range of finite concentration, its fluorescence intensity is directly proportional to arsenic content,
Compare quantitative with standard series.
1.2 instruments and reagent
AFS-820 type dual channel atomic fluorescence photometers（Beijing Jida Swan Instruments Co., Ltd）, as hollow cathode lamp（Beijing
Non-ferrous metal studies total institute）.
Arsenic standard reserving solution：GBW(E)080215（China National Measuring Science Research Inst. produces）, the concentration of this standard reserving solution
It is 100 ug/mL（Specific compound method is with described in GB GB/T 5750-2006）.
Arsenic standard working solution：As required, the ug/mL standard working solutions containing arsenic 0.1 are prepared with above-mentioned arsenic standard reserving solution,
It is stored in standby in polyethylene bottle.
Thiourea and ascorbic acid mixed solution：Weigh 2.5 g thiocarbamides and 2.5 g ascorbic acid be dissolved in 100 mL ultra-pure waters,
Shake up standby.
Potassium borohydride and potassium hydroxide solution：Weigh 20 g potassium borohydrides and 5 g potassium hydroxide are dissolved in 1000 mL distilled water
In, shake up, it is stored in standby in polyethylene bottle.
Hydrochloric acid：Measure 25 mL pure hydrochloric acids（Ultra-clean extra pure regent）, it is slowly added into the distilled water of 400 mL or so, and
With distilled water diluting to 500 mL.
1.3 experimental techniques
1.3.1 the preparation of sample solution
The mL of water sampling 10, adds 1.0 mL reducing agents（The mixed solution of thiourea and ascorbic acid, thiocarbamide and anti-bad in mixed solution
The mass concentration of hematic acid is 2.5%）, 1.0 mL pure hydrochloric acids are added, it is well mixed, 40 min are placed in 100 DEG C of water-baths to be carried out
Digestion process, digestion records surplus solution volume after terminating, and sample solution is shaken up to obtain, while doing blank test.
1.3.2 the preparation of standard series
1.0 mL reducing agents are added in a series of 10 mL colorimetric cylinders（The mixed solution of thiourea and ascorbic acid, mixed solution
The mass concentration of middle thiocarbamide and ascorbic acid is 2.5%）, then be separately added into 0.1 ug/mL arsenic standard working solution 0.02,
0.05th, 0.1,0.3,0.6 and 1.2 mL, then adds 1.0 mL pure hydrochloric acids, and being finally settled to scale with ultra-pure water obtains arsenic
Standard liquid, shakes up stand-by.
1.3.3 determine
Atomic fluorescence spectrophotometer is opened, circuit, gas circuit, each system of water route is connected, by argon gas（Purity >=99.99%）Amount
Regulation opens atomic fluorescence spectrophotometer software to 0.2~0.3 MPa, is input into various parameters（Concrete numerical value is with GB GB/T
Described in 5750-2006）, fluorescence photometer is then carried out into cleaning preheating, after after instrument stabilizer, start bioassay standard curve.
With fluorescence intensity as ordinate, standard curve is drawn by abscissa of arsenic standard standard liquid concentration.Its linear regression side
Journey is If=96.1060*C-25.1688, and coefficient correlation is 0.9999, it follows that the measurement result stabilization of this experiment, i.e.,
Can determination sample.
1.3.4 calculate
With the fluorescence intensity of institute's test sample product, the arsenic concentration in sample solution is checked in from standard curve or regression equation（ug/L）.
1.3.5 the degree of accuracy
Choose 1 ug/L, 5 ug/L and 20 ug/L, tri- parts of different arsenic standard solutions are measured, obtain following result（Table 1）.
The determination of recovery rates result of table 1
| Sample number into spectrum | Treatment | The actual arsenic content of arsenic standard liquid（ug/L） | Arsenic standard liquid measures arsenic content（ug/L） | The rate of recovery（%） |
| 1 | Digestion | 1 | 1.03 | 103.00 |
| 2 | Digestion | 5 | 5.01 | 100.20 |
| 3 | Digestion | 20 | 19.38 | 96.90 |
As seen from Table 1, the measurement result of 1 ug/L, 5 ug/L and 20 ug/L arsenic standard liquids is respectively 1.03 ug/L, 5.01
Ug/L and 19.38 ug/L, the rate of recovery meets measure and requires 96.9%~103%, illustrates the present invention to arsenic content in water
Method it is feasible.
2 control experiments
In order to verify that the inventive method determines the validity and accuracy of arsenic content in water, using three kinds of methods respectively to 38 parts of water
Sample carries out arsenic content, and 38 parts of water samples are mainly in the collection of the ground such as Shaanxi, Guangxi and Yunnan.
Experimental technique 1（GB GB/T 5750-2006 methods）With method 2（The inventive method）Use same AFS-
820 type dual channel atomic fluorescence photometers are measured；Method 3（ICP-MS）Directly produced using PerkinElmer companies
ICP-MS instruments are measured.
The result of the total arsenic content in three kinds of method measure water is as shown in table 2：
2 three kinds of method arsenic content results of table
Note：SY is water sample
From table 2, three kinds of method measurement results have difference, but the measurement result of method 2 and method 3 is very identical, 33 water
The measurement result for having more than 10 in sample is closely such as SY1, SY2, SY3 and SY6 etc.（Table 1）；And use method 1
Although measurement result it is consistent with the trend of method 2, the measurement result of method 3, can also reflect and to determine arsenic content in water sample
Height changes, but measurement result is more unstable, and many sample determination results are higher, such as SY-2, SY-4, SY-5, SY-8 and SY-16
Deng, especially SY-22 and SY-23, its measurement result compared with method 2, method 3, up to more than hundred times unexpectedly of difference.Thus see
Go out, the advantages of the inventive method has cost-effective, data are reliable.
Claims (5)
1. in a kind of water arsenic content assay method, it is characterised in that comprise the following steps：
（1）Sample solution is prepared, process for preparation is：Water sample, reducing agent, pure hydrochloric acid are mixed, mixed solution is obtained, then
Mixed solution heating is carried out into digestion process, digestion records surplus solution volume, shakes up after terminating, and obtains sample solution, while
Do blank test；The reducing agent for thiourea and ascorbic acid mixed solution, and in mixed solution thiocarbamide and ascorbic acid matter
Amount concentration is 2.5%；
（2）Prepare arsenic standard solution；
（3）Sample solution is introduced into atomic fluorescence spectrophotometer, the fluorescence intensity of arsenic in determination sample solution, according to concentration known
The fluorescence intensity that arsenic standard solution is measured calculates the content of arsenic in sample solution.
2. in a kind of water according to claim 1 arsenic content assay method, it is characterised in that：Step（1）Middle water sample, also
Former agent, pure hydrochloric acid are with 10:1:1 volume ratio is mixed.
3. in a kind of water according to claim 1 arsenic content assay method, it is characterised in that：Step（1）Middle heating disappears
Changing the condition for the treatment of is：Mixed solution places 40 min under 100 DEG C of water-baths.
4. in a kind of water according to claim 1 arsenic content assay method, it is characterised in that：Step（1）Described in sulphur
The compound method of urea-ascorbic acid mixed solution is：Weigh 2.5 g thiocarbamides and 2.5 g ascorbic acid are dissolved in 100 mL ultra-pure waters
In, shake up standby.
5. in a kind of water according to claim 1 arsenic content assay method, it is characterised in that：Step（1）In match somebody with somebody sample preparation
Detailed process during product solution is：The mL of water sampling 10, adds 1.0 mL reducing agents, adds 1.0 mL pure hydrochloric acids, and mixing is equal
It is even, 40 min are placed under 100 DEG C of water-baths, surplus solution volume is recorded, shake up to obtain sample solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108776125A (en) * | 2018-08-03 | 2018-11-09 | 贵州省疾病预防控制中心 | A kind of sample pre-treatments reagent and method measured in urine during arsenic |
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| US3897155A (en) * | 1972-08-04 | 1975-07-29 | Unisearch Ltd | Atomic fluorescence spectrometer |
| CN1415957A (en) * | 2001-11-02 | 2003-05-07 | 中国石油天然气股份有限公司 | Method for detecting content arsenic in water |
| CN104076016A (en) * | 2014-07-09 | 2014-10-01 | 中蓝连海设计研究院 | Method for measuring content of arsenic in phosphate ore |
| 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 |
-
2016
- 2016-12-28 CN CN201611237805.3A patent/CN106770118A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3897155A (en) * | 1972-08-04 | 1975-07-29 | Unisearch Ltd | Atomic fluorescence spectrometer |
| CN1415957A (en) * | 2001-11-02 | 2003-05-07 | 中国石油天然气股份有限公司 | Method for detecting content arsenic in water |
| CN104076016A (en) * | 2014-07-09 | 2014-10-01 | 中蓝连海设计研究院 | Method for measuring content of arsenic in phosphate ore |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108776125A (en) * | 2018-08-03 | 2018-11-09 | 贵州省疾病预防控制中心 | A kind of sample pre-treatments reagent and method measured in urine during arsenic |
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Application publication date: 20170531 |