CN104677900A - Method capable of eliminating influence of reagent blank and rapidly detecting content of chlorine dioxide in water - Google Patents

Method capable of eliminating influence of reagent blank and rapidly detecting content of chlorine dioxide in water Download PDF

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CN104677900A
CN104677900A CN201510090771.9A CN201510090771A CN104677900A CN 104677900 A CN104677900 A CN 104677900A CN 201510090771 A CN201510090771 A CN 201510090771A CN 104677900 A CN104677900 A CN 104677900A
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chlorine dioxide
color
reagent
water
blank
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CN104677900B (en
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林林
连国军
黄陈平
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Wenzhou Medical University
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Abstract

The invention discloses a method capable of eliminating the influence of a reagent blank and rapidly detecting the content of chlorine dioxide in water. The method comprises the following steps: firstly, preparing a liquid-type chlorine dioxide detection reagent, then manufacturing a chlorine-dioxide standard color card without the reagent blank by a colorless and transparent PVC (Polyvinyl Chloride) plastic board, putting the chlorine-dioxide standard color card at the bottom part of a blank tube in testing, and reading the concentration of chlorine dioxide corresponding to the standard color card when the color is consistent to that of a sample tube, thereby obtaining the concentration of chloride dioxide in a water sample. The method disclosed by the invention has the advantages that if the method is adopted for carrying out detection on the concentration of chloride dioxide, the influence of the reagent blank on a detection result can be eliminated, and the method is especially suitable for on-site fast detection of chloride dioxide in water.

Description

A kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact
Technical field
The present invention relates to field of water quality detection, particularly relate to a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact.
Background technology
Chlorine dioxide (ClO 2) be efficient, the wide spectrum of the latest generation of generally acknowledging in the world at present, the sterilization of safety, antistaling agent, be the optimal substitute of chlorinated product, be widely used at World Developed Countries.The teratogenesis easily produced when using the Drinking Water of chlorine dioxide treatment can not produce the chlorine-containing disinfectants such as usual sodium hypochlorite, cause change, carcinogenic methenyl choloride, but skin contact or the solution taken in containing high concentration of chlorine dioxide, still may cause intense stimulus and corrosive attack.
In water, the detection of chlorine dioxide adopts the spectrophotometric method that directly develops the color, Fading spectrophotometry, fluorimetry, chemical titration, chromatography, electrochemical method, plasma resonance scattering method more, these methods all need water sample to take back special laboratory, chemically examined by the operative technique personnel of specialty, the large-scale instrumentation that major part method also needs price high, quick, easy Site Detection requirement can not be met, some special when and wheres also exist sampling not in time, the situation of sampling location Water quality can not be objectively responded.
Existing chlorine dioxide Site Detection reagent is the dry-type detection reagent based on colourimetry in the market, this detection reagent get when measuring a certain amount of water sample and dry-type detect reagent mix, dissolve, react a period of time after produce specific color, directly contrast the concentration drawing water sample test substance with standard color card.These class methods fast, convenient, public participation degree is high, but cannot eliminate the impact of change on measurement result of reagent blank when measuring, and only just has higher accuracy when reagent blank is invariable.But actual detection finds, be no matter the detection reagent of liquid-type or dry-type, in storing process, all inevitably there is reagent blank become situation that is large or that diminish gradually.In addition, when using the detection reagent of dry-type to carry out water sample detection, need first fully to dissolve detecting reagent with water sample to be measured, then carry out reaction with the concrete pollutant in water sample and produce particular color.Because the TWS of Various Seasonal, zones of different collection is not quite similar, during dissolving dry-type detection reagent, required time is also not quite similar, and whole testing process required time is difficult to effective control, also causes adverse effect to the accuracy of testing result.
Therefore, demand is a kind of uses liquid-type to detect reagent, can eliminate reagent blank on testing result impact, use the direct visual colorimetric determination of standard color card quantitative water in the detection method of chlorine dioxide, seem particularly important for realizing chlorine dioxide field quick detection in water.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, the invention provides a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact.
For achieving the above object, the present invention adopts following scheme: a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact, is characterized in that described method comprises the steps:
(1) liquid-type chlorine dioxide detects the preparation of reagent, and described liquid-type chlorine dioxide detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.19-0.38 mmol/L
Glycocoll 0.267-0.675 mol/L
Disodium ethylene diamine tetraacetate 2.69-5.38 mmol/L
Ethylene glycol 0.36-0.90 mol/L
PH6.50 phosphate buffer 30-80 mmol/L;
(2) preparation of the chlorine dioxide standard color card after reagent blank is deducted, be taken to few 4 color comparison tubes, optional 1 color comparison tube is blank tube, residue color comparison tube is standard pipe, first deionized water is added in blank tube, the chlorine dioxide standard solution of concentration in gradient change is first added in each standard pipe, the deionized water added in blank tube is identical with the chlorine dioxide standard solution volume added in standard pipe, the liquid-type chlorine dioxide detection reagent that the step (1) of same volume is obtained is added in all color comparison tubes, reaction to color no longer changes, by bottom color comparison tube in each color comparison tube of photographs be color, with mapping software by each standard pipe color deduction blank tube color, again the concentration of the chlorine dioxide standard solution of the color of gained and correspondence is printed on water white transparency plate,
(3) detection of water sample to be measured, be taken to few 2 color comparison tubes simultaneously, optional 1 color comparison tube is blank tube, all the other color comparison tubes are sample hose, first deionized water is added in blank tube, water sample to be measured is first added in sample hose, the deionized water added in blank tube is identical with the volume of water sample to be measured added in sample hose, the liquid-type chlorine dioxide detection reagent that the step (1) of same volume is obtained is added in all color comparison tubes, reaction to color no longer changes, then standard color card made for step (2) is placed in bottom blank tube, observe the overlay color of blank tube and chlorine dioxide standard color card, read chlorine dioxide concentration overlay color corresponding to the most close with sample hose color.
As preferred version of the present invention, the liquid-type chlorine dioxide in step (1) detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.26-0.31 mmol/L
Glycocoll 0.37-0.57 mol/L
Disodium ethylene diamine tetraacetate 3.74-4.34 mmol/L
Ethylene glycol 0.53-0.73 mol/L
PH6.50 phosphate buffer 40-65 mmol/L.
As present invention further optimization, the liquid-type chlorine dioxide in step (1) detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.28 mmol/L
Glycocoll 0.471 mol/L
Disodium ethylene diamine tetraacetate 4.04 mmol/L
Ethylene glycol 0.63 mol/L
PH6.50 phosphate buffer 50 mmol/L.
As preferred version of the present invention, 7 color comparison tubes are got in step (2), an optional color comparison tube is blank tube, adds the chlorine dioxide standard solution that concentration is 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L, 0.80mg/L in all the other six roots of sensation color comparison tubes successively.
As preferred version of the present invention, the water white transparency PVC plastic flitch of water white transparency plate to be thickness be 1-2mm.
Good effect of the present invention is as follows:
The method eliminating chlorine dioxide content in the quick detection water of reagent blank impact of the present invention has the advantage that method is simple, accuracy is high, be easy to operation; Use liquid-type chlorine dioxide to detect reagent to detect, effectively can control whole testing process required time; By blank tube color addition is carried out the method for colorimetric control with sample hose again on standard color card, effectively can eliminate the impact of reagent blank on testing result, be particularly suitable for chlorine dioxide field quick detection in water.
Embodiment
Embodiment 1
(1) liquid-type chlorine dioxide detects the preparation of reagent, and described liquid-type chlorine dioxide detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.19 mmol/L
Glycocoll 0.267 mol/L
Disodium ethylene diamine tetraacetate 2.69 mmol/L
Ethylene glycol 0.36 mol/L
PH6.50 phosphate buffer 30 mmol/L;
(2) preparation of the chlorine dioxide standard color card after reagent blank is deducted, get 7 10ml glass color comparison tubes, arranging the 1st color comparison tube is blank tube, 2-7 root color comparison tube is standard pipe, 10ml deionized water is added respectively and 10ml concentration is 0.05mg/L in blank tube and standard pipe, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L, the chlorine dioxide standard solution of 0.80mg/L, the liquid-type chlorine dioxide added again described in step (1) detects reagent 0.2ml, react under room temperature to color and no longer change, by bottom color comparison tube to the color that each tube reaction of photographs produces, with mapping software photoshop7.0 by after each standard pipe color deduction blank tube color, the concentration of the chlorine dioxide standard solution of the color of gained and correspondence is printed on the water white transparency PVC plastic flitch that thickness is 1mm,
(3) 2 10ml glass color comparison tubes are got, arranging the 1st color comparison tube is blank tube, 2nd color comparison tube is sample hose, 10ml deionized water and 10ml water sample to be measured is added respectively in blank tube and sample hose, add the liquid-type chlorine dioxide described in step (1) again and detect reagent, react under room temperature to color and no longer change, standard color card described in step (2) is placed in bottom the blank tube of this step, by upwards observe bottom blank tube blank tube superpose with standard color card after color, and with sample hose color comparator, when both solid colours, read chlorine dioxide concentration overlay color corresponding to the most close with sample hose color.
Embodiment 2
(1) liquid-type chlorine dioxide detects the preparation of reagent, and described liquid-type chlorine dioxide detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.28 mmol/L
Glycocoll 0.471 mol/L
Disodium ethylene diamine tetraacetate 4.04 mmol/L
Ethylene glycol 0.63 mol/L
PH6.50 phosphate buffer 50 mmol/L;
(2) preparation of the chlorine dioxide standard color card after reagent blank is deducted, get 7 10ml glass color comparison tubes, arranging the 1st color comparison tube is blank tube, 2-7 root color comparison tube is standard pipe, 10ml deionized water is added respectively and 10ml concentration is 0.05mg/L in blank tube and standard pipe, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L, the chlorine dioxide standard solution of 0.80mg/L, the liquid-type chlorine dioxide added again described in step (1) detects reagent 0.2ml, react under room temperature to color and no longer change, by bottom color comparison tube to the color that each tube reaction of photographs produces, with mapping software photoshop7.0 by after each standard pipe color deduction blank tube color, the concentration of the chlorine dioxide standard solution of the color of gained and correspondence is printed on the water white transparency PVC plastic flitch that thickness is 1mm,
(3) 2 10ml glass color comparison tubes are got, arranging the 1st color comparison tube is blank tube, 2nd color comparison tube is sample hose, 10ml deionized water and 10ml water sample to be measured is added respectively in blank tube and sample hose, add the liquid-type chlorine dioxide described in step (1) again and detect reagent, react under room temperature to color and no longer change, standard color card described in step (2) is placed in bottom the blank tube of this step, by upwards observe bottom blank tube blank tube superpose with standard color card after color, and with sample hose color comparator, when both solid colours, read chlorine dioxide concentration overlay color corresponding to the most close with sample hose color.
Embodiment 3
(1) liquid-type chlorine dioxide detects the preparation of reagent, and described liquid-type chlorine dioxide detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.38 mmol/L
Glycocoll 0.675 mol/L
Disodium ethylene diamine tetraacetate 4.04 mmol/L
Ethylene glycol 0.90 mol/L
PH6.50 phosphate buffer 80 mmol/L;
(2) preparation of the chlorine dioxide standard color card after reagent blank is deducted, get 7 10ml glass color comparison tubes, arranging the 1st color comparison tube is blank tube, 2-7 root color comparison tube is standard pipe, 10ml deionized water is added respectively and 10ml concentration is 0.05mg/L in blank tube and standard pipe, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L, the chlorine dioxide standard solution of 0.80mg/L, the liquid-type chlorine dioxide added again described in step (1) detects reagent 0.2ml, react under normal temperature to color and no longer change, by bottom color comparison tube to the color that each tube reaction of photographs produces, with mapping software photoshop7.0 by after each standard pipe color deduction blank tube color, the concentration of the chlorine dioxide standard solution of the color of gained and correspondence is printed on the water white transparency PVC plastic flitch that thickness is 1mm,
(3) 2 10ml glass color comparison tubes are got, arranging the 1st color comparison tube is blank tube, 2nd color comparison tube is sample hose, 10ml deionized water and 10ml water sample to be measured is added respectively in blank tube and sample hose, add the liquid-type chlorine dioxide described in step (1) again and detect reagent, react under normal temperature to color and no longer change, standard color card described in step (2) is placed in bottom the blank tube of this step, by upwards observe bottom blank tube blank tube superpose with standard color card after color, and with sample hose color comparator, when both solid colours, read chlorine dioxide concentration overlay color corresponding to the most close with sample hose color.
Embodiment 4
In order to verify effect of the present invention further, investigate the change of reagent blank to the impact of measurement result accuracy, invention has been following contrast test: detecting reagent by the method obtaining liq type chlorine dioxide described in this law embodiment 1 step (1) is test group, not deduct reagent blank, the detection reagent adopting standard color card direct color comparison is control group, two group reagents are put respectively 4 DEG C of refrigerators and 37 water-baths store 7 days, and measure with the water sample that national standard method mensuration chlorine dioxide concentration is 0.05mg/L with a, replace water sample to carry out reagent blank test with deionized water simultaneously, by 721 spectrophotometer record reagent blank values, the results are shown in Table 2.
Table 2
As can be seen from Table 2, under identical experiment condition, along with the increase gradually of reagent blank, the measurement result of test group remains unchanged, but the measurement result of control group obviously becomes large, show that method of the present invention effectively can remove the change of reagent blank to the impact of chlorine dioxide test result.
The present invention is not limited to above-mentioned embodiment; persons skilled in the art, according to content disclosed by the invention, adopt other multiple embodiments to implement of the present invention, or every employing thinking of the present invention; do simple change or change, all fall into protection scope of the present invention.

Claims (6)

1. can eliminate a method for chlorine dioxide content in the quick detection water of reagent blank impact, it is characterized in that described method comprises the steps:
(1) liquid-type chlorine dioxide detects the preparation of reagent, and described liquid-type chlorine dioxide detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution,
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.19-0.38 mmol/L
Glycocoll 0.267-0.675 mol/L
Disodium ethylene diamine tetraacetate 2.69-5.38 mmol/L
Ethylene glycol 0.36-0.90 mol/L
PH6.50 phosphate buffer 30-80 mmol/L;
(2) preparation of the chlorine dioxide standard color card after reagent blank is deducted, be taken to few 4 color comparison tubes, optional 1 color comparison tube is blank tube, residue color comparison tube is standard pipe, under 5-40 DEG C of condition, first deionized water is added in blank tube, the chlorine dioxide standard solution of concentration in gradient change is first added in each standard pipe, the deionized water added in blank tube is identical with the chlorine dioxide standard solution volume added in standard pipe, the liquid-type chlorine dioxide detection reagent that the step (1) of same volume is obtained is added in all color comparison tubes, reaction to color no longer changes, by bottom color comparison tube in each color comparison tube of photographs be color, with mapping software by each standard pipe color deduction blank tube color, again the concentration of the chlorine dioxide standard solution of the color of gained and correspondence is printed on water white transparency plate,
(3) detection of water sample to be measured, be taken to few 2 color comparison tubes simultaneously, optional 1 color comparison tube is blank tube, all the other color comparison tubes are sample hose, under 5-40 DEG C of condition, first deionized water is added in blank tube, water sample to be measured is first added in sample hose, the deionized water added in blank tube is identical with the volume of water sample to be measured added in sample hose, the liquid-type chlorine dioxide detection reagent that the step (1) of same volume is obtained is added in all color comparison tubes, reaction to color no longer changes, then standard color card made for step (2) is placed in bottom blank tube, observe the overlay color of blank tube and chlorine dioxide standard color card, read chlorine dioxide concentration overlay color corresponding to the most close with sample hose color.
2. a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact according to claim 1, it is characterized in that: the liquid-type chlorine dioxide in step (1) detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.26-0.31 mmol/L
Glycocoll 0.37-0.57 mol/L
Disodium ethylene diamine tetraacetate 3.74-4.34 mmol/L
Ethylene glycol 0.53-0.73 mol/L
PH6.50 phosphate buffer 40-65 mmol/L.
3. a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact according to claim 1, it is characterized in that: the liquid-type chlorine dioxide in step (1) detects reagent, by substance withdrawl syndrome, following component and deionized water is configured to solution
(N, N-diethyl-Isosorbide-5-Nitrae-phenylenediamine) sulfate 0.28 mmol/L
Glycocoll 0.471 mol/L
Disodium ethylene diamine tetraacetate 4.04 mmol/L
Ethylene glycol 0.63 mol/L
PH6.50 phosphate buffer 50 mmol/L.
4. a kind of method eliminating chlorine dioxide content in the quick detection water of reagent blank impact according to claim 1 or 2 or 3, it is characterized in that: in step (2), get 7 color comparison tubes, an optional color comparison tube is blank tube, adds the chlorine dioxide standard solution that concentration is 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L, 0.80mg/L in all the other six roots of sensation color comparison tubes successively.
5. a kind of according to claim 1 or 2 or 3 eliminates the method for chlorine dioxide content in the quick detection water of reagent blank impact, it is characterized in that: the water white transparency PVC plastic flitch of water white transparency plate to be thickness be 1-2mm.
6. according to claim 4ly a kind ofly eliminate the method for chlorine dioxide content in the quick detection water of reagent blank impact, it is characterized in that: the water white transparency PVC plastic flitch of water white transparency plate to be thickness be 1-2mm.
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