CN105823745B - Chromium scene Emergent detection reagent and its application method in a kind of water body - Google Patents
Chromium scene Emergent detection reagent and its application method in a kind of water body Download PDFInfo
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- CN105823745B CN105823745B CN201610172319.1A CN201610172319A CN105823745B CN 105823745 B CN105823745 B CN 105823745B CN 201610172319 A CN201610172319 A CN 201610172319A CN 105823745 B CN105823745 B CN 105823745B
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses chromium scene Emergent detection reagent and its application methods in a kind of water body, utilize chromium（Ⅵ）In acid condition with diphenylcarbazide（DPC）Chromogenic reaction prepare color developing agent, utilize ceric sulfate chromium oxide in acid condition（Ⅲ）Oxidation reaction prepare oxidant, selection sodium azide is reducing agent, and application method is as follows：One, when measuring chromium in water sample（Ⅵ）When concentration, color developing agent I is added in 5mL water samples to be measured, 10mL is settled to after dissolving, stands 10min, is measured to get chromium in water sample to be measured using portable spectrophotometer（Ⅵ）Concentration；Two, when measuring total chromium concn in water sample, oxidant A is added in 5mL water samples to be measured, water sample is in faint yellow, 1 ~ 2 drop reducing agent B of dropwise addition takes off to faint yellow after standing 10 ~ 15min, color developing agent II is added, it is settled to 10mL, uses spectrophotometric determination to get total chromium concn in water sample to be measured after standing 10min.The present invention has many advantages, such as that high sensitivity, accuracy are good, timeliness is strong, easy to carry.
Description
Technical field
The invention belongs to technical field of analysis and detection, it is related to chromium scene Emergent detection reagent and its user in a kind of water body
Method.
Background technology
Sudden water pollution event refers to that leakage is polluted caused by human factor or natural phenomena, is caused in the short time
Water body accommodates a large amount of pollutants and causes water quality deterioration phenomenon, and this phenomenon has not only broken up water body normal function, more serious shadow
Socio-economic development is rung.Common pollutant includes acid, alkali, organic matter, heavy metal, algae, oils, biological species etc..Wherein
Heavy metal pollution be known as toxicity is big, pollution sources extensively, be easily bioaccumulation and have the features such as biological amplification, easily to environment
Cause irreversible harm.Heavy metal chromium is mainly used for intermetallic composite coating, leather industry, electroplating industry etc., the discharge of these industrial departments
Waste water be chromium in water pollution main source.Chromium（Ⅵ）It for the property swallowed poisonous substance/imbedibility poisonous substance, is easily absorbed by the body, can lead to
Alimentary canal, respiratory tract, skin and mucous membrane intrusion human body are crossed, causes inherited genetic defects even carcinogenic, has lasting danger to environment
It is dangerous.The things that take place frequently such as Shuangfeng County's pollution of chromium of Hunan Loudi, the smeltery's pollution of chromium of the Hunan pools Xin Hualang, Qujing of Yunnan be chromium slag contaminated
Part has focused concern of the society to pollution of chromium in water body.
Chromium common detection methods include precision instrument method and spectrophotometry etc. in water body.Above method accuracy is high, smart
Exactness is good, but it not only needs expensive large scale equipment, and detection process is complicated, and cost is higher, is limited only to laboratory
Analysis.To realize that chromium Site Detection in water, the detection method research based on analytical technology, biotechnology and information technology have obtained
Significant progress, wherein what is quickly grown includes stripping voltammetry and biochemical process.At the same time, some are light, simple, easy
In carrying detecting instrument also facing market, such as test paper method, testing cassete method, portable spectrophotometer method.It is wherein portable
Spectrophotometer test is simple, and easy to carry, performance is relatively stable, in conjunction with chromium（Ⅵ）Common color developing agent diphenylcarbazide
（DPC）The fast-field evaluation of chromium can be realized.Diphenyl carbazide spectrophotometry is used based on lab analysis in national standard,
It just can be used for live Emergent detection after improvement.Liu Wenxia is mentioned substitutes acetone with ethyl alcohol, and the color developing agent holding time can be made longer；
Solid developer, high sensitivity and the interference that can shelter iron ion is made in DPC and sodium fluoride by Luo Yan etc..You Tiexue etc. is only added
1+1 phosphoric acid not only increases the sensitivity of method, more expands the range of linearity of working curve.In terms of total chromium mark feed, national standard
Middle selection potassium permanganate oxidation method, heating use sodium azide or urea-sodium nitrite reduction again after boiling 10min；Cao Guiping etc.
Select potassium chlorate be used as oxidant, measure chromate waste water mean concentration and National Standard Method without significant difference；Fan Yuanyuan etc. was used
Ammonium sulfate oxidizing process, method detection limit reach 0.003mg/L, and accuracy is higher.Poomrat Rattanarat etc. are measuring air
In particulate matter when soluble chromium, with ceric sulfate to chromium（Ⅲ）Aoxidized, at normal temperatures reaction can carry out, oxidation effectiveness compared with
It is good.
But the above research is suitable for lab analysis.Up to now, it does not find DPC, ceric sulfate, Azide
Sodium etc. is distributed into reagent, and achievable chromium is made（Ⅵ）, total chromium on-site measurement detection kit relevant report.
Invention content
It is existing that the object of the present invention is to provide chromium in a kind of high sensitivity, the water body that accuracy is good, timeliness is strong, easy to carry
Field Emergent detection reagent and its application method, suitable for measuring chromium surface water, underground water, drinking water, industrial or agricultural water（Ⅵ）、
Total chromium.
The purpose of the present invention is what is be achieved through the following technical solutions：
Chromium scene Emergent detection reagent in a kind of water body, including color developing agent I, color developing agent II, oxidant A and reducing agent B tetra-
Part, sealing is for use respectively, wherein：
The color developing agent I is suitable for chromium（Ⅵ）Detection, prepares in accordance with the following methods：In parts by weight, by DPC1 ~ 2 part,
20 ~ 30 parts of mixing of sodium chloride, are ground into solid developer；Weigh above-mentioned 0.1 ~ 0.3g of solid developer, be added 1+1 phosphoric acid 0.1 ~
0.2mL, 0.5 ~ 0.8mL of ethyl acetate are mixed into 1mL reagents with deionized water, obtain color developing agent I.
Most preferably, by weight, by 20 parts of DPC1 parts, sodium chloride mixing, it is ground into solid developer；It weighs above-mentioned
Solid developer 0.2g is added 1+1 phosphoric acid 0.1mL, ethyl acetate 0.5mL, is mixed into 1mL reagents with deionized water, must develop the color
Agent I.
The color developing agent II is detected suitable for total chromium, is prepared in accordance with the following methods：0.1 ~ 0.3g of solid developer is weighed, is added
Enter 0.5 ~ 0.8mL of ethyl acetate and be mixed into 1mL reagents with deionized water, obtains color developing agent II.
Most preferably, solid developer 0.2g is weighed, ethyl acetate 0.5mL is added, 1mL examinations are mixed into deionized water
Agent obtains color developing agent II.
The oxidant A is prepared in accordance with the following methods：In parts by weight, 4 ~ 5 parts of ceric sulfate, deionized water 1000 are taken
Part, it is configured to ceric sulfate solution；Above-mentioned 50 ~ 60mL of solution is taken, 1+1 0 ~ 12mL of phosphatase 11 are added, is dissolved by heating, is taken after cooling
0.1 ~ 0.2mL solution is made into 1mL reagents with deionized water, obtains oxidant A.
Most preferably, in parts by weight, 4 parts of ceric sulfate, 1000 parts of deionized water is taken to be made into ceric sulfate solution；
Above-mentioned solution 50mL is taken, and 10mL1+1 phosphoric acid heating for dissolving is added, 0.1mL solution is taken to be made into 1mL examinations with deionized water after cooling
Agent obtains oxidant A.
The reducing agent B is prepared in accordance with the following methods：By weight, take 2 ~ 3 parts of sodium azide, deionized water 1000 ~
1500 parts, it is configured to sodium azide solution, 50 ~ 60mL is taken to be fitted into bottle, obtains reducing agent B.
Most preferably, by weight, 2 parts of sodium azide, 1000 parts of deionized water are taken, sodium azide solution is configured to,
50mL is taken, reducing agent B is obtained.
Above-mentioned diphenylcarbazide, sodium chloride, ethyl acetate, ceric sulfate, sodium azide are commercially available analysis pure chemistry
Product, 1+1 phosphoric acid are that 85% concentrated phosphoric acid prepares gained in equal volume with deionized water.
The application method of above-mentioned detection reagent, includes the following steps：
One, when measuring chromium in water sample（Ⅵ）When concentration, color developing agent I is added in 5mL water samples to be measured, is settled to after dissolving
10mL stands 10min, is measured to get chromium in water sample to be measured using portable spectrophotometer（Ⅵ）Concentration；
Two, when measuring total chromium concn in water sample, oxidant A is added in 5mL water samples to be measured, water sample is quiet in faint yellow
1 ~ 2 drop reducing agent B of dropwise addition takes off to faint yellow after setting 10 ~ 15min, and color developing agent II is added, is settled to 10mL, after standing 10min
With spectrophotometric determination to get total chromium concn in water sample to be measured.
Above-mentioned water sample to be measured refers to surface water, underground water, drinking water, industrial or agricultural water containing chromium.
Above-mentioned chromium refers to chromium（Ⅵ）, total chromium.
The present invention utilizes chromium（Ⅵ）In acid condition with diphenylcarbazide（DPC）Chromogenic reaction prepare color developing agent,
Utilize ceric sulfate chromium oxide in acid condition（Ⅲ）Oxidation reaction prepare oxidant, selection sodium azide is reducing agent.
Compared with the prior art, the invention has the advantages that：
1, chromium can be achieved at the same time in detection reagent of the invention（Ⅲ）, chromium（Ⅵ）, total chromium assay, when use be not required to plus
Heat, it is easy to operate, it is easy to carry about with one.
2, detection reagent high sensitivity of the invention, detection range are 0.02 ~ 1.0mg/L, are suitable for surface water, underground
The live Emergent detection of content of chromium ion in the water bodys such as water, drinking water, industrial or agricultural water.
3, detection reagent stability of the invention is good, and reagent long shelf-life, color developing agent I, II is under 4 DEG C of shading air-proof conditions
It can be stabilized 1 month or more, other reagent shelf-lifves are at least at 1 year or more.
Description of the drawings
Fig. 1 is the assembling detection kit structure diagram according to embodiment 1 and embodiment 2；
Fig. 2 is to measure chromium according to the detection reagent that the determination step of embodiment 3, embodiment 4 is drawn（Ⅵ）Application method letter
Figure（Determining instrument is by taking PF-12 portable spectrophotometers as an example）；
Fig. 3 is to measure total chromium application method schematic diagram according to the detection reagent that the determination step of embodiment 5, embodiment 6 is drawn
（Determining instrument is by taking PF-12 portable spectrophotometers as an example）.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, however, it is not limited to this, every right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit of the technical scheme of the invention and range, should all be contained
It covers in protection scope of the present invention.
Embodiment 1
Prepare chromium（Ⅵ）Detection reagent：1g diphenylcarbazides, 20g sodium chloride are weighed, mixed grinding uniformly obtains solid
Color developing agent；It measures 50mL85% phosphoric acid to mix with 50mL deionized waters, obtains 1+1 phosphoric acid；0.2g solid developers are weighed, are added
0.1mL1+1 phosphoric acid, 0.5mL ethyl acetate mix to 1mL with deionized water, obtain color developing agent I.
Embodiment 2
Prepare total chromium detection reagent：0.2g solid developers are weighed, 0.5mL ethyl acetate is added, is mixed with deionized water
To 1mL, color developing agent II is obtained；0.404g ceric sulfates are weighed, are dissolved in 50mL deionized waters, 10mL1+1 phosphoric acid is added and adds
Heat of solution takes 0.1mL solution to be made into 1mL reagents with deionized water, obtains oxidant A after cooling；0.2g sodium azide is weighed, is dissolved
Reducing agent B is obtained in 100mL deionized waters.
Above-mentioned diphenylcarbazide, sodium chloride, ethyl acetate, ceric sulfate, sodium azide are commercially available analysis pure chemistry
Product.
Embodiment 3
The chromium that embodiment 1 using the present invention obtains（Ⅵ）Detection reagent measures chromium in Song Hua River simulation low stain water sample
（Ⅵ）Concentration.
Song Hua River water sample takes 5mL in teat glass after filter paper filters, and the chromium of 10mg/L is added into test tube（Ⅵ）Mark
Quasi- solution 0.1mL simulates low concentration pollution water sample.Color developing agent I is added（1mL is filled）And 10mL is added water to, after rocking uniformly, stand
10min, using spectrophotometer wavelength be 540nm place measure absorbance, substitution chromium（Ⅵ）Standard curve calculating concentration, 6 times
Measurement result is respectively：0.117,0.117,0.119,0.117,0.118,0.116mg/L, relative standard deviation 0.88% are returned
Yield is 97.67%.The result measured with National Standard Method is 0.120mg/L, and numerical value difference is smaller, and therefore, which measures chromium
（Ⅵ）As a result accurate, reliable.
Embodiment 4
The chromium that embodiment 1 using the present invention obtains（Ⅵ）Detection reagent measures the chromium of Song Hua River simulation high pollution water sample
（Ⅵ）Concentration.
Song Hua River water sample takes 5mL in teat glass after filter paper filters, and 100mg/L chromium is added into test tube（Ⅵ）Storage
Standby solution 0.08mL, simulates high density pollution water sample.Color developing agent I is added（1mL is filled）, 10mL is added water to, uniform standing is rocked
Absorbance is measured after 10min at 540nm, 6 times measurement result is as follows：0.821、0.819、0.818、0.817、0.819、
0.818mg/L, relative standard deviation are that 0.17% rate of recovery is 99.92%.National Standard Method measured value is 0.820mg/L, numerical value difference
Less, therefore, the reagent measured value is accurate and reliable.
Embodiment 5
It is dense that total chromium detection reagent that embodiment 2 using the present invention obtains measures total chromium in Song Hua River simulation low concentration water sample
Degree.
Song Hua River water sample after filtering, takes 5mL in teat glass, and the chromium of 10mg/L is added into test tube（Ⅵ）Standard is molten
Liquid 0.1mL simulates low concentration pollution water sample.Oxidant A is added, water sample is in faint yellow, 10 ~ 15min of standing after mixing, dropwise addition 1 ~
2 drop reducing agent B take off to faint yellow.Color developing agent II is added, mixing measures absorbance after standing 10min at 540nm, measures 6
Secondary concentration value is as follows：0.131,0.128,0.127,0.129,0.131,0.128mg/L, relative standard deviation 1.30%, recycling
Rate is 101.17%, and the result 0.130mg/L measured with ICP-AES is very nearly the same, therefore, measures total chromium when low concentration pollution
Detection reagent is effective, reliably.
Embodiment 6
It is dense that total chromium detection reagent that embodiment 2 using the present invention obtains measures total chromium in Song Hua River simulation high concentration water sample
Degree.
Song Hua River water sample takes 5mL in teat glass after filter paper filters, and 100mg/L chromium is added into test tube（Ⅵ）Storage
Standby solution 0.08mL, simulates high density pollution water sample.Oxidant A is added, water sample is in faint yellow, and 10 ~ 15min is stood after mixing,
1 ~ 2 drop reducing agent B is added dropwise to take off to faint yellow.Color developing agent II is added, mixing measures absorbance after standing 10min at 540nm,
It is as follows to measure 6 concentration values：0.836,0.830,0.831,0.835,0.833,0.833mg/L, relative standard deviation are
0.27%, the rate of recovery 100.60% is not much different with ICP-AES measured values 0.830mg/L, therefore, measures total chromium of high concentration
Detection reagent is reliable when concentration.
Claims (9)
1. chromium scene Emergent detection reagent in a kind of water body, it is characterised in that the reagent is by color developing agent I, color developing agent II, oxidation
Agent A and tetra- parts reducing agent B are constituted, wherein：
The color developing agent I is prepared in accordance with the following methods：In parts by weight, by 1 ~ 2 part of diphenylcarbazide, sodium chloride 20 ~ 30
Part mixing, is ground into solid developer；Above-mentioned 0.1 ~ 0.3g of solid developer is weighed, 1+1 0.1 ~ 0.2mL of phosphoric acid, acetic acid is added
0.5 ~ 0.8mL of ethyl ester is mixed into 1mL reagents with deionized water, obtains color developing agent I；
The color developing agent II is prepared in accordance with the following methods：0.1 ~ 0.3g of solid developer is weighed, 0.5 ~ 0.8mL of ethyl acetate is added
1mL reagents are mixed into deionized water, obtain color developing agent II；
The oxidant A is prepared in accordance with the following methods：In parts by weight, 4 ~ 5 parts of ceric sulfate, 1000 parts of deionized water are taken,
It is configured to ceric sulfate solution；It takes above-mentioned 50 ~ 60mL of solution, 1+1 0 ~ 12mL of phosphatase 11 is added, dissolve by heating, take 0.1 after cooling ~
0.2mL solution is made into 1mL reagents with deionized water, obtains oxidant A；
The reducing agent B is prepared in accordance with the following methods：By weight, 2 ~ 3 parts of sodium azide, deionized water 1000 ~ 1500 are taken
Part, it is configured to sodium azide solution, 50 ~ 60mL is taken to be fitted into bottle, obtains reducing agent B.
2. chromium scene Emergent detection reagent in a kind of water body according to claim 1, it is characterised in that the color developing agent I is pressed
It is prepared according to following methods：By weight, by 20 parts of 1 part of diphenylcarbazide, sodium chloride mixing, it is ground into solid developer；
Above-mentioned solid developer 0.2g is weighed, 1+1 phosphoric acid 0.1mL, ethyl acetate 0.5mL is added, 1mL examinations are mixed into deionized water
Agent obtains color developing agent I.
3. chromium scene Emergent detection reagent in a kind of water body according to claim 1, it is characterised in that the color developing agent II
It prepares in accordance with the following methods：Solid developer 0.2g is weighed, ethyl acetate 0.5mL is added, 1mL examinations are mixed into deionized water
Agent obtains color developing agent II.
4. chromium scene Emergent detection reagent in a kind of water body according to claim 1, it is characterised in that the oxidant A is pressed
It is prepared according to following methods：In parts by weight, 4 parts of ceric sulfate, 1000 parts of deionized water is taken to be made into ceric sulfate solution；It takes
Above-mentioned solution 50mL, and 10mL1+1 phosphoric acid heating for dissolving is added, take 0.1mL solution to be made into 1mL examinations with deionized water after cooling
Agent obtains oxidant A.
5. chromium scene Emergent detection reagent in a kind of water body according to claim 1, it is characterised in that the reducing agent B is pressed
It is prepared according to following methods：By weight, 2 parts of sodium azide, 1000 parts of deionized water are taken, sodium azide solution is configured to, takes
50mL obtains reducing agent B.
6. chromium scene Emergent detection reagent in water body according to claim 1, it is characterised in that the diphenylcarbazide,
Sodium chloride, ethyl acetate, ceric sulfate, sodium azide are commercially available analysis pure chemicals.
7. chromium scene Emergent detection reagent in water body according to claim 1, it is characterised in that the 1+1 phosphoric acid is 85%
Concentrated phosphoric acid prepares gained in equal volume with deionized water.
8. the application method of chromium scene Emergent detection reagent in the water body described in a kind of claim 1 ~ 7 any claim,
Being characterized in that the method, steps are as follows：
One, when measuring VI concentration of chromium in water sample, color developing agent I is added in 5mL water samples to be measured, 10mL is settled to after dissolving, it is quiet
10min is set, is measured to get VI concentration of chromium in water sample to be measured using portable spectrophotometer；
Two, when measuring total chromium concn in water sample, oxidant A is added in 5mL water samples to be measured, water sample in faint yellow, stand 10 ~
1 ~ 2 drop reducing agent B is added dropwise after 15min to take off to faint yellow, color developing agent II is added, is settled to 10mL, light splitting is used after standing 10min
Photometric determination is to get total chromium concn in water sample to be measured.
9. the application method of chromium scene Emergent detection reagent in water body according to claim 8, it is characterised in that described to wait for
It refers to surface water, underground water, drinking water or industrial or agricultural water containing chromium to survey water sample.
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| CN107084935A (en) * | 2017-06-21 | 2017-08-22 | 佛山科学技术学院 | A kind of quick determination method of chromium ion |
| CN111077090B (en) * | 2019-12-10 | 2020-09-11 | 中国环境科学研究院 | Cr in soil containing large amount of reducing agent6+Is detected by |
| CN111610184A (en) * | 2020-05-26 | 2020-09-01 | 王淑娟 | Semi-quantitative detection method for total residual chlorine in water |
| CN111610183A (en) * | 2020-05-26 | 2020-09-01 | 王淑娟 | Semi-quantitative detection method for total residual chlorine in wastewater |
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