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CN102033063A - Preparation and use method of color comparison detection piece for ammonia nitrogen in water - Google Patents

Preparation and use method of color comparison detection piece for ammonia nitrogen in water Download PDF

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Publication number
CN102033063A
CN102033063A CN201010524008XA CN201010524008A CN102033063A CN 102033063 A CN102033063 A CN 102033063A CN 201010524008X A CN201010524008X A CN 201010524008XA CN 201010524008 A CN201010524008 A CN 201010524008A CN 102033063 A CN102033063 A CN 102033063A
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Prior art keywords
ammonia nitrogen
color comparison
water
color
detection piece
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郜洪文
贾江雁
郜子蕙
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SHANGHAI LVDIST ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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SHANGHAI LVDIST ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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Abstract

The invention relates to a preparation and use method of a color comparison detection piece for ammonia nitrogen in water, in particular to a color comparison detection piece and method for semi-quantitative detection of concentration of ammonia nitrogen in water bodies. The detection piece comprises a development upper layer containing tetraiodomercurate compounds, an inert isolation layer and a reaction lower layer containing alkali and masking agents, the detection piece is prepared into a three-layer piece by pressing, and the detection piece needs to be saved in sealing and light-shielding environment and can be used effectively within 4 months. The use method comprises the following steps: directly immersing the detection piece into 10ml of water sample, joggling a color comparison cup for 10-30 minutes, comparing the color of the upper layer of the piece with the color of a standard color comparison card of ammonia nitrogen (concentration: 0-20.0mg/L), and then, estimating the concentration of the ammonia nitrogen in the water sample. The color comparison detection piece for ammonia nitrogen developed by the invention can be used for quickly detecting the concentration of the ammonia nitrogen in water bodies such as surface water, domestic sewage, industrial waste water and the like without adding any reagent. The piece has long effective period and low price and can be carried conveniently. The invention provides the simple, convenient and practical method for quickly detecting the ammonia nitrogen in mountain areas, remote areas, oceans, industrial pollution sources and the like on the site.

Description

A kind of preparation and using method of water quality ammonia nitrogen color comparison detection lug
Technical field
The present invention relates to a kind of preparation and application process thereof that detects the colorimetric detection sheet of ammonia nitrogen in the water body, belong to the environmental monitoring technology field.
Background technology
Along with the fast development of industrial technology, Sudden Pollution Accident constantly increases, and is threatening human health, is destroying ecologic environment, is seriously restricting the ecologic equilibrium and society, expanding economy.It is a lot of to take precautions against burst Pollution accident problem demanding prompt solution, top priority is to set up the emergency monitoring method and technology, in case contamination accident takes place, can drop into monitoring rapidly, in the shortest time, provide contamination data accurately, for antipollution diffusion and take counter-measure that scientific basis is provided.Therefore, extremely strong for time and spatial character, the significant Sudden Pollution Accident of random variation, on-the-spot detection obtain in time and answer comparatively accurately to detect accurate perfect answer than a laboratory of coming too lately valuable many.In-situ check and test method normally detects in real time in the workplace, promptly records whether have test substance and concentration thereof in the sample at short notice.Being used for the on-the-spot method that detects, to need sampling quantity few, and possess characteristics such as higher accuracy and sensitivity, the instrument that fast, uses easy and simple to handle are easy to carry.Comparatively ripe at present in-situ check and test method has test paper method, detector tube method, micro-titration method, Bioexperiment method, portable instrument method etc.
Water quality ammonia nitrogen detection method mainly contains Na Shi reagent method, salicylic acid spectrophotometric method, distillation-neutralization titration, indigo colourimetry, flow analysis and spectrum detection method, ion-selective electrode etc.The complex operation that these methods have, analytical cycle is long, and the liquid reagent developing time is long and stabilization time short; The instrument of the needs costliness that has is had relatively high expectations to operating personnel's professional skill, can only finish in the laboratory, can not satisfy the requirement of fast-field evaluation.For this reason, numerous researchers have carried out many improvement and innovation, especially at the scene the fast detecting aspect.Long Xiwei etc. take to add in the flow injection system method of gas disperser, allow the ammonia nitrogen in the water sample see through gas separation membrane after generating ammonia for the reaction of NaOH carrier fluid, in bromine thymol blue absorption liquid, react variable color again, use spectrophotometry, the result shows, concentration and absorbance are favorable linearity in 0~50mg/L interval, its related coefficient is 0.995, measure ammonia-nitrogen content in the water body, the recovery reach 99% (Long Xiwei, Wu Ting, Li Fang etc. the online detection of flow injection spectrophotometric method of ammonia nitrogen in the water. the naval vessel chemical defence, 2008, (2): 34-37).Zhu Ke waits ammonia nitrogen determination method in the Drinking Water that adopts the ion-selective electrode method to succeed in developing the use of a kind of suitable basic unit clearly, measure 3 parts of synthetic water samples, relative standard deviation is 0.50%~2.44%, detection limit (3 δ) 0.032mg/L, the recovery 95.0%~106.7%, that this method has is simple to operate, quick, accurate, disturb advantages such as few, stronger (the Zhu Keqing of practicality, Xie Peng. ammonia nitrogen in the ion-selective electrode method Drinking Water. straits preventive medicine magazine, 2009,15 (4): 54-55).Hou Chuanjia etc. utilize the method for gas phase uv absorption Fourier transform to develop water quality ammonia nitrogen in-line analyzer, this method selectivity height when measuring surface water and waste water, almost do not disturb, advanced technology, rational in infrastructure, have the remote transmission function, simultaneously this still is the instrument of a modular, can measure 12 parameters of as many as.Compare with classic method, have that maintenance is little, operating cost is low, anti-colourity and turbidity disturb, need not to mark every day advantages such as calibration solution (Hou Chuanjia, Wang Xin. a kind of gas phase uv absorption Fourier transform water quality ammonia nitrogen in-line analyzer of novelty. modern instrument, 2008, (2): 50-53).Nie Xuejun etc. have designed a kind of based on Na Shi reagent colourimetry moral ammonia nitrogen determination instrument, this instrument has the distillation pretreatment unit, can detect the ammonia-nitrogen content in any water sample, and be to carry out data acquisition and processing (DAP) automatically, the mensuration of ammonia-nitrogen content in the quick realization water (Nie Xuejun, Zhou Feng, Huo Liangsheng etc. the research and development of full-automatic ammonia nitrogen determination instrument. microcomputer information, 2009,25 (1): 129-130).The improvement that above-mentioned researcher is done water quality ammonia nitrogen fast-field evaluation method all is instrumental methods, and test paper method research is very few.Deng Jinhua etc. adopt the total solids mix reagent, improved salicylic acid spectrophotometric method are applied to the mensuration of water quality ammonia nitrogen.The maximum absorption wavelength of complex compound is 697nm, the ammonia nitrogen mass concentration meets Beer law between 0.01~1.00mg/L, the reaction product color keeps stablizing all interference measurements not of common coexisting ion in 3h, the fast measuring that can be used for the ambient water quality ammonia nitrogen, though have a lot of problems in this method practical application, but the test paper method that detects to the water quality ammonia nitrogen steps the (Deng Jinhua that goes a step further, Wu Qingping, Liao Fuying etc. the fast detecting of ambient water quality ammonia nitrogen. environmental monitoring management and technology, 2007,19 (1): 33-34).
Summary of the invention
The purpose of this invention is to provide and a kind ofly portably use conveniently, cheap be suitable for the tablet that environment water ammonia-nitrogen contents such as surface water, sanitary sewage, industrial waste water detect.By the detection lug colour developing depth and ammonia nitrogen concentration correlativity, realize ammonia nitrogen concentration in the water body is carried out semiquantitative method for quick.
In order to achieve the above object, the present invention utilizes the classical detection method of ammonia nitrogen: Na Shi reagent method, preparation water quality ammonia nitrogen detection lug.Concrete preparation method is as follows:
This water quality ammonia nitrogen color comparison detection lug closes the color layer that mercury meets thing, the responding layer that contains alkali and screening agent by containing the tetraiodo, and color layer and the separated inert layer of responding layer are formed.
The preparation method of described ammonia nitrogen color comparison detection lug is: the tetraiodo is closed mercury compound, inert material and bonding agent and is mixed with 1: 8: 1~5: 4: 1 ratio, uses as the colour developing upper layer of material.Mix with inert material and bonding agent ratio, as the intermediate isolating layer material with 9: 1~6: 4.Mix with inorganic sodium, NaOH and sodium potassium tartrate tetrahydrate ratio, as the reaction subsurface material with 1: 1: 1~3: 1: 1.Get down 0.5~1g responding layer material, 0.5~1g isolate in layer material, 0.3~0.5g colour developing upper layer of material put into the sheeter mould of diameter 8~20mm successively, compression molding when pressure is 5~30MPa promptly gets the ammonia nitrogen color comparison detection lug.
The above-mentioned tetraiodo is closed mercury compound preparation method: get 0.02mol aluminium nitrate, 0.01mol potassium mercuric iodide, 0.2mol NaOH or potassium hydroxide, adding 500mL does not have ammoniacal liquor, as solution A.Get 0.04~0.08mol magnesium nitrate, adding 250mL does not have ammoniacal liquor, as solution B.Use separating funnel that solution B is slowly splashed into solution A, regulate pH to 9~10, and be settled to 1L, stirring reaction two hours, centrifugal after with wet slag in 120 ℃ of drying boxes dry 4 hours.
Above-mentioned inertia medicament is commercially available analytical pure sulfuric acid calcium or nano double oxyhydroxide.
Above-mentioned binder is commercially available polynite, paraffin, ethyl cellulose, methylcellulose.
Above-mentioned inorganic sodium is the commercially available pure sodium carbonate of analysis, sodium sulphate, sodium nitrate.
Above-mentioned potassium mercuric iodide is a chemical pure; It is pure that aluminium nitrate, magnesium nitrate, NaOH, potassium hydroxide, tartrate clock sodium are analysis.
The making and methods for using them of water quality ammonia nitrogen examination criteria colorimetric card is:
A, standard color comparison card is made
Be respectively 0~20.0mg/L ammonia nitrogen standard series with the ammonium chloride compound concentration, respectively get 10 milliliters, under 25 ℃, the colorimetric detection sheet is soaked in wherein, shakes cuvette, after 15 minutes, press concentration series arrangement from low to high, take, make the ammonia nitrogen standard color comparison card with high definition camera.
B, ammonia nitrogen detects in the water sample
The colorimetric detection sheet is directly immersed~10 milliliters of water samples to be measured in, make color layer up, shake cuvette, take out after 10~20 minutes, with its colour developing upper strata and standard color comparison card color contrast, ammonia nitrogen concentration in the sample estimates.
Advantage of the present invention is:
Since water quality ammonia nitrogen color comparison detection lug of the present invention by three-deckers such as color layer, separation layer, dissolving layers, do not need to add in addition any reagent during use, have portably use conveniently, cheap characteristics, detecting for mountain area, backcountry, ocean, pollution source are on-the-spot etc. provides fast and practical approach.
2. the colorimetric detection sheet is solid-state tri-layer tablets, and the design of separation layer has improved the stability of reactant.
3 are somebody's turn to do than color chips sensing range: 0~20mg/L ammonia nitrogen is suitable for the detection of ammonia nitrogen in the various water bodys such as surface water, sanitary sewage, industrial waste water.
Embodiment
Embodiment 1
Ammonia nitrogen examination criteria colorimetric card is made
Use that the ammonium chloride compound concentration is respectively 0,0.50,1.0,2.0,3.0,5.0,10.0,20.0mg/L ammonia nitrogen standard solution, under 25 ℃, get 10 milliliters of above-mentioned solution respectively in eight 20ml glass cells, the ammonia nitrogen color comparison detection lug is soaked wherein, behind the 15min, arrange from low to high according to ammonia nitrogen concentration, take pictures and make standard color comparison card, as table 1.
Table 1 water quality ammonia nitrogen standard color comparison card
Figure BSA00000324063400041
Embodiment 2
The experiment of colorimetric detection tablet stability
At ambient temperature, the sealing, the ammonia nitrogen color comparison detection lug keeps in Dark Place, when preserving 5,10,20,30,60,90,120 days, respectively to 0,2.0,10.0mg/L ammonia nitrogen solution measures, the result shows: when different time, the detection lug color of same ammonia nitrogen concentration does not have significant difference, and therefore, it is effective that this ammonia nitrogen detection lug used in 4 months.
Embodiment 3
The ammonia nitrogen of actual water sample detects
Get 10 milliliters of West Lake water and TAIHU LAKE respectively in cuvette, detection lug is soaked in wherein, take out detection lug behind the 15min, with its upper strata color and standard color comparison card contrast, in the sample estimates concentration of ammonia nitrogen be respectively 0.3,0.7mg/L, and use Na Shi reagent method, laboratory operation to record that the West Lake and TAIHU LAKE are respectively 0.269, the 0.648mg/L ammonia nitrogen, both are unanimity as a result, shows this water quality ammonia nitrogen color comparison detection lug mensuration accurately.

Claims (4)

1. the preparation and the using method of a water quality ammonia nitrogen color comparison detection lug is characterized in that, by containing the reaction lower floor that the tetraiodo is closed the colour developing upper strata of mercury compound, contained alkali and screening agent, and the inert barriers that will connect levels forms, and adds compressed tablets by sheeter.During use, directly the colorimetric detection sheet directly is soaked in the water sample, behind the certain hour, upper strata color and the comparison of ammonia nitrogen standard color comparison card, ammonia nitrogen concentration in the semiquantitative determination sample.
2. the preparation method of the described water quality ammonia nitrogen color comparison of claim 1 detection lug is characterized in that: the tetraiodo is closed mercury compound, inert material, bonding agent mix with 1: 8: 1~5: 4: 1 ratio, grind, as the tablet upper layer of material.Inert material, bonding agent are mixed with 9: 1~6: 4 ratio, grind, as the intermediate isolating layer material.Inorganic sodium, alkali, sodium potassium tartrate tetrahydrate are mixed with 1: 1: 1~3: 1: 1 ratio, grind, as the tablet subsurface material.Use pressed disc method, get 0.5~1g subsurface material, 0.5~1g insolated layer materials, 0.3~0.6g upper layer of material, will descend, in, the upper strata powder adds sheeter successively, be forced into 5~30MPa, make thickness 4~6mm, diameter 8~20mm tablet, sealing, black out are preserved, and use effectively in 4 months.
3. the described tetraiodo of claim 1 is closed mercury compound preparation method and is: get 0.02mol aluminium nitrate, 0.01mol potassium mercuric iodide, 0.2mol NaOH or potassium hydroxide, join after the mixing in the 500mL deionized water, as solution A.Get 0.04~0.08mol magnesium nitrate and join the 250mL deionized water, as solution B.Under agitation, solution B is slowly splashed into solution A, regulates terminal point pH9~10, be settled to 1L, stirred again two hours, centrifugal after with wet slag in 120 ℃ of drying boxes dry 4 hours.
Above-mentioned inert material is commercially available analytical pure sulfuric acid calcium or magnalium double-hydroxide.
Above-mentioned bonding agent is commercially available polynite, paraffin, ethyl cellulose, methylcellulose.
Above-mentioned inorganic sodium is the commercially available pure sodium carbonate of analysis, sodium sulphate, sodium nitrate.
Above-mentioned potassium mercuric iodide is a chemical pure; It is pure that aluminium nitrate, magnesium nitrate, NaOH, potassium hydroxide, sodium potassium tartrate tetrahydrate are analysis.
4. the preparation and the using method of the ammonia nitrogen standard color comparison card of claim 1 is characterized in that:
(1) the ammonia nitrogen standard color comparison card is made
With ammonium chloride compound concentration 0~20mg/L ammonia nitrogen standard series, under 25 ℃, the colorimetric detection sheet is placed in 10 ml solns, hybrid reaction 15 minutes is arranged from low to high by ammonia nitrogen concentration, takes with high definition camera and makes the ammonia nitrogen standard color comparison card.
(2) ammonia-nitrogen content detects in the actual water body
The ammonia nitrogen color comparison detection lug is immersed in~10 milliliters of water samples to be measured, make color layer up, take out to develop the color upper strata and standard color comparison card color contrast, ammonia nitrogen concentration in the direct estimation sample after 10~30 minutes.
CN201010524008XA 2010-10-28 2010-10-28 Preparation and use method of color comparison detection piece for ammonia nitrogen in water Pending CN102033063A (en)

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN102879241A (en) * 2011-07-13 2013-01-16 上海绿帝环保科技有限公司 Rapid phosphate detection tablet
CN103018187A (en) * 2012-12-10 2013-04-03 同济大学 Method for preparing and using color developing detection sheet for measuring hydrazine in water
CN103033503A (en) * 2012-12-10 2013-04-10 同济大学 Preparation and application method of chromogenic detecting piece for determining iron in water
CN103776826A (en) * 2014-01-16 2014-05-07 无限极(中国)有限公司 Masking-agent-containing test strip for detecting content of cadmium in Chinese herbal medicine
CN104374771A (en) * 2014-11-19 2015-02-25 阜阳师范学院 Kit for rapidly detecting ammonia nitrogen content in water and detection method of kit
CN104535503A (en) * 2015-01-14 2015-04-22 同济大学 Method for preparing and using detection agent for measuring content of cobalt in water body
CN104568936A (en) * 2015-01-12 2015-04-29 河北工业大学 Ammonia nitrogen test paper and application method thereof
CN104614328A (en) * 2014-11-17 2015-05-13 上海明华电力技术工程有限公司 Method for determining ammonia content of fly ash or sediment
CN107132216A (en) * 2016-02-29 2017-09-05 福建大北农水产科技有限公司 A kind of breeding water body ammonia nitrogen quick detection kit

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102879241A (en) * 2011-07-13 2013-01-16 上海绿帝环保科技有限公司 Rapid phosphate detection tablet
CN103018187A (en) * 2012-12-10 2013-04-03 同济大学 Method for preparing and using color developing detection sheet for measuring hydrazine in water
CN103033503A (en) * 2012-12-10 2013-04-10 同济大学 Preparation and application method of chromogenic detecting piece for determining iron in water
CN103776826A (en) * 2014-01-16 2014-05-07 无限极(中国)有限公司 Masking-agent-containing test strip for detecting content of cadmium in Chinese herbal medicine
CN103776826B (en) * 2014-01-16 2016-05-25 无限极(中国)有限公司 With the test strips of the detection Chinese herbal medicine cadmium content of screening agent and in the purposes detecting in Chinese herbal medicine cadmium content
CN104614328A (en) * 2014-11-17 2015-05-13 上海明华电力技术工程有限公司 Method for determining ammonia content of fly ash or sediment
CN104374771A (en) * 2014-11-19 2015-02-25 阜阳师范学院 Kit for rapidly detecting ammonia nitrogen content in water and detection method of kit
CN104568936A (en) * 2015-01-12 2015-04-29 河北工业大学 Ammonia nitrogen test paper and application method thereof
CN104568936B (en) * 2015-01-12 2018-01-09 河北工业大学 A kind of ammonia nitrogen Test paper and its application process
CN104535503A (en) * 2015-01-14 2015-04-22 同济大学 Method for preparing and using detection agent for measuring content of cobalt in water body
CN107132216A (en) * 2016-02-29 2017-09-05 福建大北农水产科技有限公司 A kind of breeding water body ammonia nitrogen quick detection kit

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Application publication date: 20110427