CN208902512U - A kind of experimental provision of photocatalytic method resolution water sample - Google Patents
A kind of experimental provision of photocatalytic method resolution water sample Download PDFInfo
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- CN208902512U CN208902512U CN201820500184.1U CN201820500184U CN208902512U CN 208902512 U CN208902512 U CN 208902512U CN 201820500184 U CN201820500184 U CN 201820500184U CN 208902512 U CN208902512 U CN 208902512U
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Abstract
A kind of experimental provision of photocatalytic method resolution water sample, comprising: device frame body, magnetic stirring apparatus and ultraviolet lighting device；Described device frame includes pedestal, bracket and ultraviolet source cover；The magnetic stirring apparatus includes the motor being set in pedestal, the magnet to connect with motor drive shaft and control unit；The ultraviolet lighting device includes ultraviolet lamp tube and intensity of illumination regulating device.This technology can be completed entirely to clear up step at normal temperatures and pressures, avoid the high temperature and pressure resolution environment used in conventional method, improve conventional efficient, reduce the potential risk of experiment and testing cost.
Description
Technical field
The utility model relates to water quality inspection technique fields, and in particular to using the experimental provision of photocatalytic method resolution water sample
And its method.
Background technique
Since nitrogen, phosphorus are the main nutrient elements for leading to water eutrophication, therefore total nitrogen (TN), total phosphorus (TP) become weighing apparatus
Measure the important indicator of water quality.With sharply increasing for economic fast development and population, largely carry various organic matters and nitrogen,
Industrial wastewater, agricultural effluent and the sanitary sewage of the nutriments such as phosphorus are discharged into rivers,lakes and seas so that all kinds of receiving water body water quality
Increasingly deteriorate, compromise the health of the mankind.In face of water quality situation, urgent need finds a kind of effective total phosphorus, total nitrogen detection method.
Nowadays the national standard method (GB 11893-89) of total phosphorus is measured, principle is that over cure is added into a certain amount of water sample
Sour potassium (K2S2O8) solution, the heated oxide 30min at 120 DEG C, the phosphorous compound in water sample is oxidized to phosphate, cold
But to the ascorbic acid solution that 1mL is added after room temperature, 2mL ammonium molybdate solution is added after 30s, P-Mo blue is generated, in 700nm wave
Long lower measurement absorbance.
The national standard method (HJ 636-2012) of total nitrogen is measured, principle is that potassium peroxydisulfate is added into a certain amount of water sample
(K2S2O8) solution and sodium hydroxide (NaOH) solution, the heated oxide 30min at 120 DEG C contains nitrogen compound in water sample
It is oxidized to nitrate anion, after being cooled to room temperature plus hydrochloric acid is adjusted to pH value to 2~3, with ultraviolet spectrophotometry respectively at 220nm
With at 275nm survey its absorbance (A), by A=A220-2A275Calculate its absorbance.
As can be seen that the resolution of both methods requires a high-pressure relief device from principle, need in a height
It is carried out in the environment of warm high pressure, time-consuming for such digestion procedure, and temperature is difficult to control, and has security risk, and in alkaline condition
Under, the N element in water is easy to escape at high temperature, causes error to result, stability is poor.And it is surveyed using spectrophotometry
Amount, required reagent is more and reagent purity is required very high, and more many and diverse, reagent price is also costly.
Therefore, it is necessary to seek a kind of quick and easy safety resolution water sample device and method.It is required that this equipment safety, fastly
Speed, required reagent is few, at low cost.The detection method of total nitrogen and total phosphorus suitable for all kinds of water samples.
Utility model content
The purpose of this utility model is to provide a kind of experimental provision of photocatalytic method resolution water sample, can be in normal temperature and pressure
Under water sample is cleared up and is detected.
Following technical proposal can be used to realize in the purpose of this utility model: a kind of experiment dress of photocatalytic method resolution water sample
It sets, the experimental provision is made of device frame body 1, magnetic stirring apparatus 2 and ultraviolet lighting device 3；Described device frame body 1 wraps
Include pedestal 10, bracket 11 and ultraviolet source cover 12；The magnetic stirring apparatus 2 includes motor 20 and horse in pedestal 10
The magnet 21 and control unit 22 to connect up to axis；The ultraviolet lighting device 3 includes that ultraviolet lamp tube 30 and intensity of illumination adjust dress
Set 31.
The experimental provision of the photocatalytic method resolution water sample, magnetic stirring apparatus 2 is two or more, is symmetricly set on
In pedestal 10.
The experimental provision of the photocatalytic method resolution water sample, the motor 20 being set in pedestal 10, magnet 21 are two groups
More than, and it controls its revolving speed by control unit 22 respectively.
The experimental provision of the photocatalytic method resolution water sample, control unit 22 further include power switch 220 and can divide
Different groups of 2 revolving speeds of magnetic stirring apparatus are not shown and show the display screen 221 of intensity of illumination.
The technological progress of the utility model is specific as follows:
1) present apparatus uses ultraviolet photolysis, replaces the resolution of High-temperature Digestion device, can complete entirely to clear up at normal temperatures and pressures
Step avoids the high temperature and pressure resolution environment used in conventional method, sufficiently raising conventional efficient, it is potential to reduce experiment
Risk.
2) this method uses TiO2Experimental cost is reduced since it can be recycled as catalyst.It also avoids
Conventional oxidant nitrogen-containing impurity is more and influences caused by result.
3) this method uses the content of Determination of Total Nitrogen In Water By Ion Chromatography total phosphorus, reduces the preparation work of a large amount of reagents
Make, improves efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model；
Fig. 2 is the circuit control principle figure of the utility model.
Specific embodiment
Illustrate the technical scheme in the embodiment of the utility model in order to clearer, below will to case study on implementation describe in need
Attached drawing to be used is briefly described, and drawings discussed below is only some examples of the present utility model, for this
It for the different technologies personnel of field, can also be obtained according to these attached drawings other embodiments, belong to the utility model protection
Range.
Digestion instrument is sent out referring to the photocatalysis that shown in Fig. 1 and Fig. 2, the present utility model is proposed comprising ultraviolet light
Source irradiation system and magnetic agitation system.Power supply used is 220V alternating current, the ultraviolet light source irradiation system by lampshade 1,
Ultraviolet lamp 2 and bracket 10 form, and the bracket 10 is connected with pedestal 7, and wherein lampshade 1 is connected with bracket 10 by knob, convenient
It is dismantled and replacement ultraviolet lamp.The magnetic agitation system has a blender 3,4,8,9, speed regulator 5, switch 6 and 7 groups of pedestal
At adjusting the revolving speed of blender 3,4,8,9 respectively by speed regulator 5, switch 6 controls the on and off of ultraviolet lamp 2.
Measurement of the utility model for total nitrogen content in water sample, comprising the following steps:
1) a certain amount of water sample to be measured, is taken, have impurity uses membrane filtration, removes impurity；
2) deimpurity water sample to be measured, is being removed, adjusting its pH value with sulfuric acid is 8.5-9；
3) the photochemical catalyst hydrogen peroxide (H of 0.5-1%, is added by water sample weight2O2)；
4) 0.1% photochemical catalyst titanium dioxide (TiO, is added by water sample weight2)；
5) container of above-mentioned catalyst, will be added, being placed on magnetic agitating device in revolving speed is 100 turns/min, ultraviolet light
Under the conditions of source strength is 365nm, stirring, irradiation resolution 30 minutes；
6), the catalyst solid in filtering removal container in the solution through clearing up, obtains filtrate；
7), with the total amount of the nitrogen in ion-chromatographic determination filtrate, set the response condition of ion chromatograph are as follows: yin from
Sub- splitter.Carbonate leacheate, flow velocity 1.0ml/min, suppressor electric conductivity detector, continuous self-loopa reproduction suppresser, into
Sample amount 25uL；
8), each concentration that condition is measured according to response makes canonical plotting；Its method particularly includes: it is accurate respectively to move
It takes 0.00ml, 1.00ml, 2.00ml, 5.00ml, 10.0ml, 20.0ml standard solution to be placed in one group of 100ml volumetric flask, uses
Water dilution is settled to graticule, mixes.The hybrid standard series of 6 various concentrations is configured, standard series mass concentration is respectively
0.00mg/L,1.00mg/L,2.00 mg/L,5.00mg/L,10.0mg/L,20.0mg/L.It can be according to the concentration of sample
Suitable standard series concentration range.Ion chromatography is implanted sequentially according to the sequence of its concentration from low to high, record peak area (or
Person's peak height).Using the mass concentration of each ion as abscissa, peak area (or peak height) is ordinate, draws standard curve.
9), reference standard curve graph is according to gained nitrate concentration, to learn the total nitrogen content in tested water.This is practical
The novel measurement for total phosphorus content in water sample, comprising the following steps:
1) a certain amount of water sample to be measured, is taken, have impurity uses membrane filtration, removes impurity；
2) deimpurity water sample to be measured, is being removed, adjusting its pH value with sodium hydroxide is 4.5-6；
3) the photochemical catalyst hydrogen peroxide (H of 0.5-1%, is added by water sample weight2O2)；
4) 0.1% photochemical catalyst titanium dioxide (TiO, is added by water sample weight2)；
5) container of above-mentioned catalyst, will be added, being placed on magnetic agitating device in revolving speed is 100 turns/min, ultraviolet light
Under the conditions of source strength is 365nm, stirring, irradiation resolution 30 minutes；
6), the catalyst solid in filtering removal container in the solution through clearing up, obtains filtrate；
7), with the total amount of the phosphorus in ion-chromatographic determination filtrate, the response condition of ion chromatograph is set are as follows: anion
Splitter.Carbonate leacheate, flow velocity 1.0ml/min, suppressor electric conductivity detector, continuous self-loopa reproduction suppresser, sample introduction
Measure 25uL；
8), each concentration that condition is measured according to response makes canonical plotting, method particularly includes: it is accurate respectively to move
It takes 0.00ml, 1.00ml, 2.00ml, 5.00ml, 10.0ml, 20.0ml standard solution to be placed in one group of 100ml volumetric flask, uses
Water dilution is settled to graticule, mixes.The hybrid standard series of 6 various concentrations is configured, standard series mass concentration is respectively
0.00mg/L,0.50mg/L,1.00 mg/L,2.50mg/L,5.00mg/L,10.0mg/L.It can be according to the concentration of sample
Suitable standard series concentration range.Ion chromatography is implanted sequentially according to the sequence of its concentration from low to high, record peak area (or
Person's peak height).Using the mass concentration of each ion as abscissa, peak area (or peak height) is ordinate, draws standard curve.
9), reference standard curve graph is according to gained nitrate concentration, to learn the total phosphorus content in tested water.
Measurement of the utility model for total nitrogen, total phosphorus content in water sample, comprising the following steps:
1) a certain amount of water sample to be measured, is taken, have impurity uses membrane filtration, removes impurity；
2) deimpurity water sample to be measured, is being removed, adjusting its pH value with sodium hydroxide is 7；
3) the photochemical catalyst hydrogen peroxide (H of 0.5-1%, is added by water sample weight2O2)；
4) 0.1% photochemical catalyst titanium dioxide (TiO, is added by water sample weight2)；
5) container of above-mentioned catalyst, will be added, being placed on magnetic agitating device in revolving speed is 100 turns/min, ultraviolet light
Under the conditions of source strength is 365nm, stirring, irradiation resolution 30 minutes；
6), the catalyst solid in filtering removal container in the solution through clearing up, obtains filtrate；
7), with the nitrate anion and phosphorus acid ion concentration in ion-chromatographic determination filtrate, the sound of ion chromatograph is set
Answer condition are as follows: carbonate leacheate, flow velocity 1.0ml/min, suppressor electric conductivity detector, continuous self-loopa reproduction suppresser, into
Sample amount 25uL；
8), each concentration that condition is measured according to response, makes canonical plotting respectively, method particularly includes: it is quasi- respectively
Really pipetting 0.00ml, 1.00ml, 2.00ml, 5.00ml, 10.0ml, 20.0ml standard solution is placed in one group of 100ml volumetric flask
In, it is diluted with water and is settled to graticule, mix.Configure the hybrid standard series of 6 various concentrations, standard series mass concentration difference
For total nitrogen content 0.00mg/L, 1.00mg/L, 2.00mg/L, 5.00mg/L, 10.0mg/L, 20.0mg/L, total phosphorus content 0.00
The mixed standard solution of mg/L, 0.50mg/L, 1.00mg/L, 2.50mg/L, 5.00mg/L, 10.0mg/L.It can be according to tested
The suitable standard series concentration range of the concentration of sample.It is implanted sequentially ion chromatography according to the sequence of its concentration from low to high, is remembered
It records peak area (or peak height).Using the mass concentration of each ion as abscissa, peak area (or peak height) is ordinate, draws mark
Directrix curve.
9), reference standard curve graph is according to gained nitrate concentration and phosphorus acid ion concentration, to learn in tested water
Total nitrogen and phosphorus content.
Embodiment 1: certain vaccary waste water determination of total nitrogen content.Waste water is filtered with filter paper, 100 milliliters of clear liquid is taken, is placed in beaker
In, it is 10 that dilute sulfuric acid, which is added dropwise, and adjusts pH, and 0.5 gram of TiO2 photochemical catalyst and 2 milliliter of 30% hydrogen peroxide is added, is placed in magnetic agitation
Device 3 is adjusted speed regulator 5, is stirred with suitable rotational speed, is opened 40W ultraviolet lamp source 2 by switch 6 and is irradiated.Half an hour
Afterwards, stop irradiation, take out water sample from beaker, after Filtration of catalyst particle, with the nitre in ion chromatograph measurement filtrate
Acid ion concentration.Gained nitrate concentration can be converted into the total nitrogen content in characterization waste water.
Ion-chromatographic determination process: prepare 2.0,4.0,10.0,20.0,40.0mg/L standard curves, by with it is above-mentioned
Each concentration point after preparing corresponding leacheate, is entered ion chromatography, obtains standard curve by the identical processing of step.Weight simultaneously
Repetition measurement amount sample is multiple, and measuring sample concentration is 78.5 mg/L, RSD < 5%.
Embodiment 2: certain Treatment of Metal Surface factory waste water total phosphorus determination.50 milliliters of clarified wastewater water sample are taken, is placed in a beaker,
It is 6 that dilute NaOH solution, which is added dropwise, and adjusts pH, and 0.2 gram of TiO is added2Photochemical catalyst and 0.5 milliliter of 30% hydrogen peroxide, are placed in magnetic force
Blender 3 is adjusted speed regulator 5, is stirred with suitable rotational speed, is opened 16W ultraviolet lamp source 2 by switch 6 and is irradiated.Half is small
Shi Hou stops irradiation, takes out water sample from beaker, after Filtration of catalyst particle, in ion chromatograph measurement filtrate
Phosphorus acid ion concentration.
Ion-chromatographic determination process: 2.0,4.0,10.0,20.0,40.0mg/L ion-chromatographic determination process: are prepared
Each concentration point after preparing corresponding leacheate, is entered ion chromatography by processing identical with above-mentioned steps by standard curve,
Obtain standard curve.Duplicate measurements sample is multiple simultaneously, and measuring sample concentration is 18.2mg/L, RSD < 5%.
Embodiment 3: certain waste water in pharmaceutical plants total nitrogen total phosphorus measures simultaneously.100 milliliters of clear liquid are taken after waste water is filtered with filter paper,
It is placed in a beaker, it is 7 that dilute NaOH solution, which is added dropwise, and adjusts pH, 0.5 gram of TiO2 photochemical catalyst and 1 milliliter of 30% hydrogen peroxide is added,
It is placed in magnetic stirring apparatus 3, speed regulator 5 is adjusted, is stirred with suitable rotational speed, 80W ultraviolet lamp source 2 is opened by switch 6 and is carried out
Irradiation.After half an hour, stop irradiation, take out water sample from beaker, after Filtration of catalyst particle, is measured with ion chromatograph
Nitrate anion and phosphorus acid ion concentration in filtrate.Gained phosphate concentration can be converted into the total phosphorus content in characterization waste water.
Ion-chromatographic determination process: ion-chromatographic determination process: preparing phosphate concn 2.0,4.0 respectively,
10.0,20.0,40.0mg/L standard curves, 2.0,4.0,10.0,20.0,40.0mg/L standard curve of nitrate concentration, pass through
Each concentration point after preparing corresponding leacheate, is entered ion chromatography, obtains standard curve by processing identical with above-mentioned steps.
Duplicate measurements sample is multiple simultaneously, and measuring sample total phosphorus concentration is 18.1mg/L, RSD < 5%；Total nitrogen concentration is 33.2mg/L,
RSD < 5%.
Claims (4)
1. a kind of experimental provision of photocatalytic method resolution water sample, which is characterized in that the experimental provision is by device frame body (1), magnetic
Power agitating device (2) and ultraviolet lighting device (3) composition；Described device frame body (1) includes pedestal (10), bracket (11) and ultraviolet
Light source cover (12)；The magnetic stirring apparatus (2) include in pedestal (10) motor (20), the magnet that connects with motor drive shaft
(21) and control unit (22)；The ultraviolet lighting device (3) includes ultraviolet lamp tube (30) and intensity of illumination regulating device (31).
2. the experimental provision of photocatalytic method resolution water sample according to claim 1, which is characterized in that the magnetic agitation dress
(2) are set as two or more, are symmetricly set in pedestal (10).
3. the experimental provision of photocatalytic method resolution water sample according to claim 1, which is characterized in that described to be set to pedestal
(10) motor (20), magnet (21) in are more than two, and it controls its revolving speed by control unit (22) respectively.
4. the experimental provision of photocatalytic method resolution water sample according to claim 1 or 3, which is characterized in that the control is single
First (22) further include power switch (220) and can show different groups of magnetic stirring apparatus (2) revolving speeds respectively and show intensity of illumination
Display screen (221).
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| CN108593417A (en) * | 2018-04-10 | 2018-09-28 | 深圳准诺检测有限公司 | A kind of experimental provision and its method of photocatalytic method resolution water sample |
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