CN1166944C - Method for detecting content arsenic in water - Google Patents
Method for detecting content arsenic in water Download PDFInfo
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- CN1166944C CN1166944C CNB011343745A CN01134374A CN1166944C CN 1166944 C CN1166944 C CN 1166944C CN B011343745 A CNB011343745 A CN B011343745A CN 01134374 A CN01134374 A CN 01134374A CN 1166944 C CN1166944 C CN 1166944C
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Abstract
The present invention discloses a method for detecting arsenic content in water. The present invention has the detection processes that 2 portions of potassium iodide and 0.5 to 1.5 portions of thiourea are weighed and are arranged in an arsine generation bottle, 100 to 300 portions of water sample is moved in the bottle, 15 to 30 portions of concentrated hydrochloric acid is added in the bottle, and the mixture is boiled for 3 to 10 min for cooling. Meanwhile, deionized water is used as a reagent blank, and a microcoulomb arsenic detector with good calibration can detect the reagent blank and input a blank value into an instrument. Subsequently, the generation bottle is connected with the microcoulomb arsenic detector, a potassium borohydride solution is added in the arsine generation bottle, and the arsenic detector can automatically carry out reaction titration so as to detect arsenic content in the water sample. The present invention has the advantages of high detection speed, no environmental pollution and high detection result precision and can carry out batch process for the sample.
Description
Technical field
The present invention relates to arsenic Determination on content method in a kind of water, specifically adopt the method for arsenic content in the micro-coulometric determination water.
Background technology
In the prior art, the process that " microcoulomb method " measures arsenic content in the water is: get an amount of water sample and move in the arsenic hydride generation bottle, add 5ml 85% sulfuric acid, when being placed on the electric furnace heating evaporation to surplus about 1ml liquid, takes off by bottle, add the 15ml deionized water after cooling, can be connected with calibration microcoulomb arsenic apparatus well, in bottle takes place arsenic hydride, add solution of potassium borohydride bottle takes place, instrument reacts titration automatically, measures arsenic content in the water sample.Advantage highly sensitive, that detection limit is low, interference element is few that this method has.Its principle is: after water sample is concentrated with the sulfuric acid extracting, add acid potassium borohydride and make arsenic (V) or arsenic (III) be converted into AsH
3Carry by carrier gas (being generally nitrogen) then and enter titration cell, and include I in the saturated iodo-potassium bromide composite electrolyte with titration cell
2And IBr
2 -Reaction causes I
2And IBr
2 -Ion concentration reduces, the IBr of consumption
2 -Take place by anode electrolysis, measure and replenish IBr
2 -Required electric weight can be obtained the arsenic content in the water sample.This method uses electric furnace heating extracting to concentrate, and the pre-service single sample needs 1.5 hours, and detection speed is slow, can not carry out batch processing to water sample; Produce a large amount of SO in the preprocessing process
3Toxic gas, contaminated environment, the hazard analysis personnel are healthy: this method can't be eliminated the interference of antimony element to measurement result, can cause measurement result higher when containing antimony in the water sample.
Summary of the invention
The objective of the invention is provides a kind of detection speed fast by improving the pre-service to water sample, can carry out batch processing to water sample, environmentally safe, arsenic Determination on content method in the high water of testing result accuracy.
The objective of the invention is to realize by following technical solution.
Arsenic Determination on content method in a kind of water, adopt the microcoulomb arsenic apparatus, its testing process is: take by weighing 2 parts of potassium iodides, 0.5～1.5 parts of thiocarbamides place arsenic hydride that bottle takes place, pipette 100～300 parts of water samples in this bottle, 15～30 parts of the concentrated hydrochloric acids of adding concentration 36～37%, boil cooling after 3～10 minutes, do reagent blank with deionized water simultaneously, measure reagent blank and blank value is imported instrument with the good microcoulomb arsenic apparatus of calibration, after the water sample cooling bottle will take place is connected with the microcoulomb arsenic apparatus, add solution of potassium borohydride in bottle takes place arsenic hydride, arsenic apparatus reacts titration automatically, measures the arsenic content in the water sample.
Described thiocarbamide can substitute with ascorbic acid.
The boiling to place on the electric hot plate of described water sample carried out.
The inventive method has been improved the preprocessing process of water sample, and arsenic (V) is arsenic (III) in usefulness potassium iodide and thiocarbamide (or ascorbic acid) reductive water in hydrochloric acid medium, and arsenic (III) is converted into AsH under the effect of acid potassium borohydride
3, therefore need under the effect of sulfuric acid, the high temperature extracting not concentrate, promptly can directly measure with the microcoulomb arsenic apparatus.
Different acid mediums has bigger influence to the generation of arsenic hydride.Use oxalic acid or phosphoric acid, when having calcium ion to exist in the solution, can separate out calcium oxalate or calcium phosphate precipitation, influence the reduction of arsenic and the volatilization of arsenic hydride; Use dilute sulfuric acid, can cause the dimethyl arsenic generation disproportionation reaction of 2-5%, the volatility that generates arsenic hydride is reduced.With hydrochloric acid is medium, is that potassium iodide, thiocarbamide reduction arsenic (V) are the suitable condition of arsenic (III), also is that potassium borohydride reduction arsenic (III) is the suitable condition of arsenic hydride.Therefore, hydrochloric acid is the necessary medium that arsenic hydride takes place in the inventive method.
Potassium iodide has masking action to antimony, and the used potassium iodide of the inventive method again as the screening agent of antimony in the sample, has been eliminated the interference of antimony element to measurement result both as reductive agent.
The advantage that the inventive method is compared with prior art had is: do not concentrate owing to do not need to carry out the sulfuric acid extracting in the water sample preprocessing process, make the pre-service of water sample only need to finish in 15 minutes, improved detection speed; Heated and boiled to water sample can be carried out on electric hot plate, can realize the batch processing to sample; Do not produce SO in the preprocessing process
3Toxic gas has improved staff's working environment; Eliminated the interference of antimony element, improved accuracy in detection measurement result.
Embodiment
Below in conjunction with embodiment the present invention is discussed in detail.
Embodiment 1:
Water sample is handled: take by weighing the 0.2g potassium iodide, the 0.1g thiocarbamide places arsenic hydride that bottle takes place, accurately pipette water sample 20g in this bottle, add 2.4g concentrated hydrochloric acid (36～37%), place to boil on the electric hot plate after 5 minutes and take off cooling, do reagent blank with deionized water simultaneously.
Water determination: with arsenic standard specimen calibration microcoulomb arsenic apparatus, the standard specimen recovery is reached in 100 ± 5% scopes, measure reagent blank and blank value is imported instrument with the good microcoulomb arsenic apparatus of calibration.After the water sample cooling, bottle will take place be connected with the microcoulomb arsenic apparatus, and add solution of potassium borohydride in bottle takes place arsenic hydride, arsenic apparatus reacts titration automatically, measures the arsenic content in the water sample.Arsenic content different water sample 1#, 2#, 3# are distinguished replication 6 times, and Precision test result sees the following form.
Table 1 Precision test result (n=6)
| The sample name | Water sample 1# | Water sample 2# | Water sample 3# |
| Mean value (ng/g) | 2.6 | 19.0 | 47.0 |
| Standard deviation (ng/g) | 0.46 | 0.76 | 1.32 |
| Relative standard deviation, % | 17.7 | 4.00 | 2.81 |
Interrelated data shows, art methods when the sample size scope during at 1～3000ng/g its relative standard deviation be 22～1%.By table 1 as seen, more than the test relative standard deviation and is better than universal method also in this scope.
Choose potable water and 3 kinds of sewage are measured respectively, simultaneously the water sample of handling with art methods is compared mensuration, two kinds of method measurement results see Table 2.As seen, two kinds of methods are better to the measurement result consistance of potable water and sewage from table 2, and relative deviation is in the error range that allows.
Two kinds of method measurement result contrasts of table 2
| The sample name | The inventive method (ng/g) | Art methods (ng/g) | Relative deviation (%) |
| Potable water | ＜1.0 | ＜1.0 | / |
| Sewage 1# | 8.2 | 8.1 | 1.2 |
| Sewage 2# | 13.6 | 14.0 | -2.9 |
| Sewage 3# | 47.0 | 47.8 | -1.7 |
Embodiment 2:
Water sample is handled: take by weighing the 0.2g potassium iodide, the 0.1g ascorbic acid places arsenic hydride that bottle takes place, pipette sewage 4# water sample 30g in this bottle, add 3.0g concentrated hydrochloric acid (36～37%), place to boil on the electric hot plate after 3 minutes and take off cooling, do reagent blank with deionized water simultaneously.
Water determination: with arsenic standard specimen calibration microcoulomb arsenic apparatus, the standard specimen recovery is reached in 100 ± 5% scopes, measure reagent blank and blank value is imported instrument with the good microcoulomb arsenic apparatus of calibration, use then with embodiment 1 identical method and carry out arsenic content in the water sample.Simultaneously the water sample of handling with art methods is compared mensuration, two kinds of method measurement results see Table 3.
Two kinds of method measurement result contrasts of table 3
| The sample name | The inventive method (ng/g) | Art methods (ng/g) | Relative deviation (% |
| Sewage 4# | 39.4 | 40.2 | -2.0 |
As seen, two kinds of methods are better to the measurement result consistance of sewage 4# from table 3, and relative deviation is in the error range that allows.
Embodiment 3:
Water sample is handled: take by weighing the 0.2g potassium iodide, the 0.15g ascorbic acid places arsenic hydride that bottle takes place, pipette 5# water sample 30g in this bottle, add 2.4g concentrated hydrochloric acid (36～37%), place to boil on the electric hot plate after 8 minutes and take off cooling, do reagent blank with deionized water simultaneously.
Water determination: with arsenic standard specimen calibration microcoulomb arsenic apparatus, the standard specimen recovery is reached in 100 ± 5% scopes, measure reagent blank and blank value is imported instrument with the good microcoulomb arsenic apparatus of calibration, then with carrying out arsenic content in the water sample as the method for embodiment 1.Simultaneously the water sample of handling with art methods is compared mensuration, two kinds of method measurement results see Table 4.
Two kinds of method measurement result contrasts of table 4
| The sample name | The inventive method (ng/g) | Art methods (ng/g) | Relative deviation (%) |
| Sewage 5# | 28.4 | 28.5 | -0.4 |
As seen, two kinds of methods are better to the measurement result consistance of sewage 4# from table 4, and relative deviation is in the error range that allows.
Employed microcoulomb arsenic apparatus is the As-1 type arsenic content instrument that Jiang Huan company produces in the above embodiment of the present invention.
Claims (3)
1. arsenic Determination on content method in the water, adopt the microcoulomb arsenic apparatus, the testing process that it is characterized in that it is: take by weighing 2 parts of potassium iodides, 0.5～1.5 parts of thiocarbamides place arsenic hydride that bottle takes place, pipette 100～300 parts of water samples in this bottle, 15～30 parts of the concentrated hydrochloric acids of adding concentration 36～37%, boil cooling after 3～10 minutes, do reagent blank with deionized water simultaneously, measure reagent blank and blank value is imported instrument with the good microcoulomb arsenic apparatus of calibration, after the water sample cooling bottle will take place is connected with the microcoulomb arsenic apparatus, add solution of potassium borohydride in bottle takes place arsenic hydride, arsenic apparatus reacts titration automatically, measures the arsenic content in the water sample.
2. arsenic Determination on content method in the water according to claim 1 is characterized in that: described thiocarbamide can substitute with ascorbic acid.
3. arsenic Determination on content method in the water according to claim 1 is characterized in that: the boiling to place on the electric hot plate of described water sample carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011343745A CN1166944C (en) | 2001-11-02 | 2001-11-02 | Method for detecting content arsenic in water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011343745A CN1166944C (en) | 2001-11-02 | 2001-11-02 | Method for detecting content arsenic in water |
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|---|---|
| CN1415957A CN1415957A (en) | 2003-05-07 |
| CN1166944C true CN1166944C (en) | 2004-09-15 |
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|---|---|---|---|
| CNB011343745A Expired - Fee Related CN1166944C (en) | 2001-11-02 | 2001-11-02 | Method for detecting content arsenic in water |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101726487B (en) * | 2008-10-16 | 2011-12-28 | 北京有色金属研究总院 | Method for analyzing arsenic in ore sample |
| CN106770118A (en) * | 2016-12-28 | 2017-05-31 | 许昌学院 | The assay method of arsenic content in a kind of water |
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