CN107505308A - A kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium - Google Patents
A kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium Download PDFInfo
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- CN107505308A CN107505308A CN201710682990.5A CN201710682990A CN107505308A CN 107505308 A CN107505308 A CN 107505308A CN 201710682990 A CN201710682990 A CN 201710682990A CN 107505308 A CN107505308 A CN 107505308A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention provides a kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium, comprises the following steps, S1：Preparation round bottom centrifuges plastic tube, and PH=7.0 sample solution 10mL is added in the round bottom centrifuges plastic tube；Two drop dimethyl diaminophenazine chloride indicator solutions are instilled, with color toner solution to yellow, complexing agent is added and is thoroughly mixed to form Hydrophobic Ionic associated matter with sample solution, shake up the pH to 5.0 for adjusting mixed solution after standing with cushioning liquid；S2：Continue the solution of Triton X 114 for adding 1mL APDCs solution and 1mL volume fractions are 20% in the sample solution obtained by step S2；Added in this technological process and mix colours, centrifuge the technical characteristics such as vibrations, temperature control, can not only ensure the more accurate of detection process, accuracy improves, and operates simply, is easy to actual processing, and will not bring larger pollution, is advantageous to popularization and application.
Description
[technical field]
It is simple to operate the present invention relates to trace element detection technical field, more particularly to a kind of accumulation ability are strong, and can be same
When detect multiple element ICP extraction detection Determination of Trace Mercury In Water, the method for cadmium.
[background technology]
Heavy metal pollution is always be concerned the problem of after industry is risen, and general heavy metal produces the model of toxicity
Enclose about between 1-10mg/L, the stronger metal of toxicity such as mercury, cadmium etc. produce the mass concentration scope of toxicity in 0.01-
Between 0.001mg/L.The source of mercury and cadmium has a lot, and such as old and useless battery contains mercury, cadmium heavy metal noxious material, if to waste and old
Battery is filled, and is elapsed over time, and the shell of battery can be corroded perforation, cause harmful substance to enter in soil, water body,
Environment is polluted；Index sewage effluent is not pressed by factory, causes Heavy Metals in Waters content overproof, mercury and cadmium can be in biologies
Cylinder accumulation, there is neurotoxicity, be generally absorbed by the body by skin, respiratory tract and alimentary canal, there is carcinogenesis, minamata disease
It is exactly one kind of mercury poisoning.
The pre-treatment and detection of heavy metal Hg, cadmium, it is at present to use traditional dithizone spectrophotometry and GB/T more
The cold atomic absorbent spectrophotometry that is mainly used in 7468-1987, GB/T 7475-1987 water-quality determinations and relevant criterion,
Atomic absorption method and atomic fluorescence method etc., which part standard method can not expire in terms of sensitivity, precision, accuracy
Sufficient trace analysis requirement, dithizone spectrophotometry because its cost is relatively low, instrument is easy to use, the degree of accuracy is higher, reappearance compared with
The advantages that good and be used widely, but regrettably this method need to use a large amount of organic solvents (chloroform) carry out
Liquid-liquid extraction, to realize concentration and separation, do not embody selectivity not only so, expend that the time is longer, wastes reagent, and chlorine
Imitative widely using can also cause certain harm and influence to environment and human body.
People start to strengthen green consciousness in recent years, and cloud point extraction (abbreviation CPE) is increasingly becoming experimenter in recent years
A kind of environment-friendly type of pro-gaze extracting process, the principle of cloud point extraction is according to hydrophobic in neutral surface active agent, hydrophilic group
The dissolution properties and cloud point phenomenon of group, by changing experiment parameter such as pH, temperature etc., separate hydrophobic, hydrophily thing from aqueous phase
A kind of analysis method of purifying of matter, it is suitable for mass production, and cloud point extraction is relative to traditional liquid-liquid extraction technology, tool
There are following several advantages：1. the scope used is wide, high from the extraction efficiency in object, enrichment times are larger；2. need not
Using poisonous and harmful organic reagent, the theory of green test is met, cost is cheap, there is higher economic benefit；It is 3. real
Test simple to operate, the time consumed is shorter；4. it is convenient etc. to be combined with instrumental method.
Inductively coupled plasma mass spectrometry (ICP-MS) has extremely low detection limit, the wider range of linearity, multielement
The advantages such as quick analysis, be generally approve in the world with wide variety of ambient water method for analyzing very small amount of element, therefore, in China
Technical field of environmental detection in using ICP-MS methods substitution other method be imperative.
Based on above mentioned problem, those skilled in the art has carried out substantial amounts of research and development and experiment, also to extract using ICP
The degree of accuracy of method detection trace element and practicality are able to fast lifting.
[content of the invention]
To overcome the problems of prior art, a kind of accumulation ability of present invention offer is strong, simple to operate, and can be simultaneously
Detect ICP extraction detections Determination of Trace Mercury In Water, the method for cadmium of multiple element.
The scheme that the present invention solves technical problem is to provide a kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium, including
Following steps,
S1：Preparation round bottom centrifuges plastic tube, and PH=7.0 sample solution is added in the round bottom centrifuges plastic tube
10mL；Two drop dimethyl diaminophenazine chloride indicator solutions are instilled, with color toner solution to yellow, complexing agent is added and is sufficiently mixed with sample solution
Hydrophobic Ionic associated matter is formed, shakes up the pH to 5.0 for adjusting mixed solution after standing with cushioning liquid；
S2：Continue to add 1mL APDCs solution and 1mL in the sample solution obtained by step S2
Volume fraction is 20% Triton X-114 solution；And it is integrally dilute to pour into the solution that deionized water centrifuges round bottom in plastic tube
Release to 20mL；The solution in plastic tube is centrifuged to round bottom using mixing plant and carries out uniform stirring, continues 10 minutes；Whole stirring
Process keeps scope of the solution temperature between 50-70 degrees Celsius；
S3：The round bottom centrifugation plastic tube for stirring completion is positioned in centrifuge and centrifuged 10 minutes with 5000r/min；Exist side by side
It is put into freezing environment and cools down 20 minutes so that solution surface activating agent is mutually adhered on tube wall as viscous liquid phase, small
Heart reversing centrifugal pipe aqueous phase discarded；
S4：The surfactant of round bottom centrifugation inside of plastic tubes in step S3 is mutually molten with the nitric acid that volume fraction is 15%
Liquid dilution, shake up；
S5：Analysis detection is carried out to the solution in step S4 using icp analysis instrument；
S6:Record detects obtained Determination of Trace Mercury In Water, the content of cadmium.
Preferably, the cushioning liquid in the step S1 is borax-boric acid mixed liquor that pH is 8.5.
Preferably, the toner in the step S1 is that volume ratio is 10:1 ammoniacal liquor and the ammoniacal liquor of redistilled water are molten
Liquid.
Preferably, the time diluted in the step S4, shaken up is no less than 20 minutes.
Preferably, APDC is complexing agent in the step S2, and Triton X-114 are surface
Activating agent.
Preferably, the cloud point extraction step will be in strict accordance with toning, tune pH value, heating, centrifugation, cooling, layering, dilution
Order carry out.
Preferably, during carrying out analysis detection to solution using icp analysis instrument in the step S5, solution is kept
Temperature range is between 35-45 degrees Celsius.
Preferably, stood in the step S1 after PH=7.0 sample solution 10mL is added during round bottom centrifuges plastic tube
20 to 30 minutes, then instill two drop dimethyl diaminophenazine chloride indicator solutions.
Compared with prior art, a kind of ICP of present invention extractions detection Determination of Trace Mercury In Water, cadmium method by using toning,
PH value, heating, centrifugation, cooling, layering, the order of dilution is adjusted to enter detection micro- in water-filling, in particular by icp analysis
Instrument carries out the determination of final constituent content, and it is special that the technologies such as toning, centrifugation vibrations, temperature control are added in this technological process
Sign, it can not only ensure the more accurate of detection process, accuracy improves, and operates simply, is easy to actual processing, and not
Larger pollution can be brought, is advantageous to popularization and application.
[brief description of the drawings]
Fig. 1 be a kind of present invention ICP extraction detection Determination of Trace Mercury In Water, cadmium method schematic flow sheet.
[embodiment]
To make the purpose of the present invention, technical scheme and advantage are more clearly understood, below in conjunction with drawings and Examples, to this
Invention is further elaborated.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, not
For limiting this invention.
Referring to Fig. 1, a kind of ICP extractions detection Determination of Trace Mercury In Water of the present invention, the method 1 of cadmium, comprise the following steps,
S1：Preparation round bottom centrifuges plastic tube, and PH=7.0 sample solution is added in the round bottom centrifuges plastic tube
10mL；Two drop dimethyl diaminophenazine chloride indicator solutions are instilled, with color toner solution to yellow, complexing agent is added and is sufficiently mixed with sample solution
Hydrophobic Ionic associated matter is formed, shakes up the pH to 5.0 for adjusting mixed solution after standing with cushioning liquid；
S2：Continue to add 1mL APDCs solution and 1mL in the sample solution obtained by step S2
Volume fraction is 20% Triton X-114 solution；And it is integrally dilute to pour into the solution that deionized water centrifuges round bottom in plastic tube
Release to 20mL；The solution in plastic tube is centrifuged to round bottom using mixing plant and carries out uniform stirring, continues 10 minutes；Whole stirring
Process keeps scope of the solution temperature between 50-70 degrees Celsius；
S3：The round bottom centrifugation plastic tube for stirring completion is positioned in centrifuge and centrifuged 10 minutes with 5000r/min；Exist side by side
It is put into freezing environment and cools down 20 minutes so that solution surface activating agent is mutually adhered on tube wall as viscous liquid phase, small
Heart reversing centrifugal pipe aqueous phase discarded；
S4：The surfactant of round bottom centrifugation inside of plastic tubes in step S3 is mutually molten with the nitric acid that volume fraction is 15%
Liquid dilution, shake up；
S5：Analysis detection is carried out to the solution in step S4 using icp analysis instrument；
S6:Record detects obtained Determination of Trace Mercury In Water, the content of cadmium.
By using toning, adjust pH value, heating, centrifugation, cooling, layering, dilution order enter it is micro- in water-filling
Detection, the determination of final constituent content is carried out in particular by icp analysis instrument, toning, centrifugation are added in this technological process
The technical characteristics such as vibrations, temperature control, it can not only ensure the more accurate of detection process, accuracy improves, and operates letter
Easily, it is easy to actual processing, and larger pollution will not be brought, is advantageous to popularization and application.
Preferably, the cushioning liquid in the step S1 is borax-boric acid mixed liquor that pH is 8.5.Using effect is good.
Preferably, the toner in the step S1 is that volume ratio is 10:1 ammoniacal liquor and the ammoniacal liquor of redistilled water are molten
Liquid.
Preferably, the time diluted in the step S4, shaken up is no less than 20 minutes.It is logical to dilute the time control shaken up
Cross after more repetition is tested what is drawn, may further ensure that the dilution effect of surfactant phase, carried for follow-up detection
For accurately detection basis.
Preferably, APDC is complexing agent in the step S2, and Triton X-114 are surface
Activating agent.
Preferably, the cloud point extraction step will be in strict accordance with toning, tune pH value, heating, centrifugation, cooling, layering, dilution
Order carry out.
Preferably, during carrying out analysis detection to solution using icp analysis instrument in the step S5, solution is kept
Temperature range is between 35-45 degrees Celsius.
Preferably, stood in the step S1 after PH=7.0 sample solution 10mL is added during round bottom centrifuges plastic tube
20 to 30 minutes, then instill two drop dimethyl diaminophenazine chloride indicator solutions.
In actual use, the gold content that detection method detects product can also be extracted by ICP, applies and is led in jewelry
Domain, and by a series of detection, finally ensure that every high-purity bright 99999 High Purity Gold ornaments gold content is equal to or more than
999.99‰。
Compared with prior art, a kind of ICP of present invention extractions detection Determination of Trace Mercury In Water, cadmium method 1 by using toning,
PH value, heating, centrifugation, cooling, layering, the order of dilution is adjusted to enter detection micro- in water-filling, in particular by icp analysis
Instrument carries out the determination of final constituent content, and it is special that the technologies such as toning, centrifugation vibrations, temperature control are added in this technological process
Sign, it can not only ensure the more accurate of detection process, accuracy improves, and operates simply, is easy to actual processing, and not
Larger pollution can be brought, is advantageous to popularization and application.
The embodiments of the present invention described above are not intended to limit the scope of the present invention.It is any in the present invention
Spirit and principle within the modifications, equivalent substitutions and improvements made etc., should be included in the claim protection model of the present invention
Within enclosing.
Claims (8)
1. a kind of ICP extractions detection Determination of Trace Mercury In Water, the method for cadmium, it is characterised in that：Comprise the following steps,
S1：Preparation round bottom centrifuges plastic tube, and the sample solution 10mL of PH=7.0 is added in the round bottom centrifuges plastic tube;Instill
Two drop dimethyl diaminophenazine chloride indicator solutions, with color toner solution to yellow, addition complexing agent is thoroughly mixed to form hydrophobic with sample solution
Property ionic associate, shake up stand after with cushioning liquid adjust mixed solution pH to 5.0；
S2：Continue to add 1mL APDCs solution and 1mL volumes in the sample solution obtained by step S2
Fraction is 20% Triton X-114 solution；And pour into deionized water and be integrally diluted to the solution in round bottom centrifugation plastic tube
20mL；The solution in plastic tube is centrifuged to round bottom using mixing plant and carries out uniform stirring, continues 10 minutes；Whole whipping process
Keep scope of the solution temperature between 50-70 degrees Celsius；
S3：The round bottom centrifugation plastic tube for stirring completion is positioned in centrifuge and centrifuged 10 minutes with 5000r/min；And immediately
It is put into freezing environment and cools down 20 minutes so that solution surface activating agent is mutually adhered on tube wall as viscous liquid phase, carefully
Reversing centrifugal pipe aqueous phase discarded；
S4：The surfactant of round bottom centrifugation inside of plastic tubes in step S3 is mutually dilute with the salpeter solution that volume fraction is 15%
Release, shake up；
S5：Analysis detection is carried out to the solution in step S4 using icp analysis instrument；
S6:Record detects obtained Determination of Trace Mercury In Water, the content of cadmium.
2. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
Cushioning liquid in S1 is borax-boric acid mixed liquor that pH is 8.5.
3. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
Toner in S1 is that volume ratio is 10:1 ammoniacal liquor and the ammonia spirit of redistilled water.
4. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
The time diluted in S4, shaken up is no less than 20 minutes.
5. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
APDC is complexing agent in S2, and Triton X-114 are surfactant.
6. a kind of ICP extraction detections Determination of Trace Mercury In Water as described in any one claim in claim 1 to 5, the side of cadmium
Method, it is characterised in that：The cloud point extraction step will be in strict accordance with toning, tune pH value, heating, centrifugation, cooling, layering, dilution
Order carry out.
7. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
During carrying out analysis detection to solution using icp analysis instrument in S5, keep the temperature range of solution 35-45 degrees Celsius it
Between.
8. a kind of ICP extractions detection Determination of Trace Mercury In Water as claimed in claim 1, the method for cadmium, it is characterised in that：The step
In S1 after the sample solution 10mL of PH=7.0 is added during round bottom centrifuges plastic tube, 20 to 30 minutes are stood, then instill two
Drip dimethyl diaminophenazine chloride indicator solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109884225A (en) * | 2019-03-07 | 2019-06-14 | 山东中医药高等专科学校 | Heavy metal biochemical detection methods in a kind of prepared slices of Chinese crude drugs |
| CN110658319A (en) * | 2019-10-17 | 2020-01-07 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metals in water |
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| CN103499537A (en) * | 2013-09-26 | 2014-01-08 | 苏州国环环境检测有限公司 | Method for determining content of zinc in mung beans by using cloud point extraction-atomic spectrum method |
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| CN106770793A (en) * | 2017-01-20 | 2017-05-31 | 烟台出入境检验检疫局检验检疫技术中心 | The method that QNS in breast or dairy products is detected using cloud point extraction liquid chromatography tandem mass spectrometry |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103499537A (en) * | 2013-09-26 | 2014-01-08 | 苏州国环环境检测有限公司 | Method for determining content of zinc in mung beans by using cloud point extraction-atomic spectrum method |
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| CN106323887A (en) * | 2016-08-05 | 2017-01-11 | 运城学院 | Method for measuring trace amount of zinc in salt through cloud point extraction-spectrophotometric method |
| CN106644994A (en) * | 2016-12-21 | 2017-05-10 | 南京大学 | Method for detecting inorganic mercury and organic mercury in water by solid-phase extraction-mercury analyzer |
| CN106770793A (en) * | 2017-01-20 | 2017-05-31 | 烟台出入境检验检疫局检验检疫技术中心 | The method that QNS in breast or dairy products is detected using cloud point extraction liquid chromatography tandem mass spectrometry |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109884225A (en) * | 2019-03-07 | 2019-06-14 | 山东中医药高等专科学校 | Heavy metal biochemical detection methods in a kind of prepared slices of Chinese crude drugs |
| CN110658319A (en) * | 2019-10-17 | 2020-01-07 | 绍兴市三合检测技术有限公司 | Method for detecting heavy metals in water |
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