CN1067739A - Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water - Google Patents
Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water Download PDFInfo
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- CN1067739A CN1067739A CN 92106462 CN92106462A CN1067739A CN 1067739 A CN1067739 A CN 1067739A CN 92106462 CN92106462 CN 92106462 CN 92106462 A CN92106462 A CN 92106462A CN 1067739 A CN1067739 A CN 1067739A
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Abstract
The full content of simple and easy, rapid assay methods of chlorine residue and specific purpose tool comprises in the water: 1. assay method: (A) reagent and reagent preparation (comprising the preparation of methyl orange standard solution and the preparation and markization of standard solutions of chlorine).(B) survey the specific operation process of chlorine residue in the water among the present invention: be survey instrument promptly with the specific purpose tool among the present invention, utilize the methyl orange dilute solution to be equal to or less than under 2 conditions, surveyed the process of chlorine residue in the water by structure and irreversible principle that energy destruction itself behind the oxychlorination takes on a red color in the pH value.2. the specific purpose tool in the assay method: (A) special special-purpose body.(B) special two ends are with sebific duct, and 90 ° of cambers are arranged, the dropper of band 5ml scale.This assay method has letter, standard, fast, honest and clean and portable advantage.
Description
The invention belongs to the analytical chemistry category.More definite saying so " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water.”
" chlorine residue " is meant water through chlorination, behind the contact certain hour, remains in " chlorine " in the water, and this " chlorine " can eliminate the hydrophily pathogenic bacteria.
Existing national standard " drinking water standard method of inspection " (GB5750-85) the middle prefered method of measuring chlorine residue is o-tolidine colorimetric method (being called for short the OT method), this method be pH value less than 1.8 acid solution in, make the reaction of chlorine residue and o-tolidine generate yellow quinoid compound, permanent with potassium dichromate-potassium chromate solution preparation of phosphate buffered solution preparation, surveying chlorine, to carry out visual colorimetric determination with the standard solution color range quantitative.There is following shortcoming in this method:
1, because o-tolidine reagent is potential carcinogen, and these method western countries forbid at present, U.S.'s " water and waste water standard test method " the 15th edition existing argumentation in 1980.
2, this method measurement result error is big.Because of its accuracy and precision difference are deleted in the standard law of the above-mentioned U.S..Cause the big main cause of error to be:
1. the chlorine residue colorimetric color range that is made into permanent (preserving 6 months) by a certain percentage with potassium dichromate-potassium chromate standard lean solution replaces standard cl concn series (Huang-yellowish-brown) approx,
2. original colourity of water sample and turbidity influence easily makes water sample and standard series tone inconsistent.
3, the main agents o-tolidine instability used of this method is seen the light deepening, and its solution is easily separated out no longer dissolving when being lower than 0 ℃;
4, the instrument of Shi Yonging, reagent and instrument are more, operating performance is also miscellaneous, and this method needs under laboratory condition (baking oven, analytical balance are arranged, volumetric flask, reagent bottle, transfer pipet, color comparison tube 50ml15 prop up etc.), reagent is minimum will be with 6 kinds, and the reagent preparation time needs more than 8 hours at least.
The objective of the invention is at the National Standard Method validation period,, seek a kind of have fast, accurate, letter, stable, cheapness and instrument simple and easy, rapid assay methods easy to carry at the problem that existing National Standard Method (OT method) exists.
Content of the present invention:
Figure of description 1 is the dedicated pipe body structure synoptic diagram in the specific purpose tool of the present invention;
Figure of description 2 is the measuring pipette structural representations in the specific purpose tool of the present invention;
Figure of description 3 is chlorine residue (mg/L) and methyl orange solution volume (ml) correlogram that the present invention surveys the chlorine residue special use.
Referring now to Figure of description 1,2,3 detailed description of the present invention is as follows:
One, specific purpose tool of the present invention:
Specific purpose tool of the present invention is made up of special-purpose body (Fig. 1) and measuring pipette (Fig. 2) two parts, that is:
1, the special-purpose body (Fig. 1) in the specific purpose tool: Fig. 1 is the special-purpose body transverse presentation structural representation of specific purpose tool.This special use body is made by colourless uniform glass, sealing two ends and smooth, and long 260 ± 10mm, internal diameter 32 ± 2mm, and have the garden column body of 100ml scale mark (Fig. 1-4); There is the water level mouth (Fig. 1-2) of high a 4～5mm, internal diameter 4～5mm on the top of this special use body transverse presentation structural representation, the right side of 100ml scale mark; The water filling gas outlet (Fig. 1-3) that high a 4～5mm, internal diameter 4～5mm are arranged on the right side of water level mouth (Fig. 1-2); Water level mouth (Fig. 1-2) is 15 ± 2mm with the centre distance of water filling gas outlet (Fig. 1-3).
2, the measuring pipette in the specific purpose tool (Fig. 2):
Referring now to accompanying drawing 2 measuring pipette is described below:
2-1, beaded glass (Fig. 2-1): D6mm, commercially available product:
2-2, sebific duct (Fig. 2-2): silicone tube or emulsion tube, long 50 ± 5mm, internal diameter 5mm, commercially available product;
2-3,5ml calibrated pipet (Fig. 2-3): the scale mark characteristics of this suction pipe are that the scale mark with distance suction pipe liquid droping port (Fig. 2-5) farthest is decided to be 0ml scale mark (Fig. 2-4), curve 90 degree and make the external diameter of pipe remain on 6～7mm to not extending to apart from 0ml scale mark (left side) 30 ± 5mm from the 0ml scale mark with the scale mark direction, is 35 ± 5mm by 90 degree pipe bent position to the suction pipe end, and suction pipe is terminal to be combined with the sebific duct that beaded glass (Fig. 2-1) is housed (Fig. 2-2); Liquid droping port (Fig. 2-a 5) end (thin end) at suction pipe is with long 20 ± 2mm, the commercially available sebific duct of internal diameter 1 ± 0.2mm (silicone tube or emulsion tube).
Two, reagent and reagent preparation:
1, the preparation of methyl orange standard solution:
Take by weighing 0.1000g methyl orange and place a beaker, add the small amount of thermal dissolved in distilled water, be cooled to normal temperature and add 20ml95%A.R ethanol again and be settled to 1L, shake up, this liquid is called stoste.Get stoste 5.00ml and place the 200ml volumetric flask, add 1+1A.R hydrochloric acid 0.5ml, doubly dilute to 200ml(40 with distilled water diluting), above-mentioned liquid should take on a red color, on 721 type spectrophotometers, record its absorption peak at 510mm, the absorbance of 1cm optical path absorption cell is 0.316～0.311, if non-this value of solution, reply stoste is done suitable adjustment.The stoste dilution of adjusting is methyl orange standard operation solution for 1 times.
2, the preparation of standard solutions of chlorine and markization:
(Puritabs is dissolved in the 500ml distilled water to take by weighing the 0.10g sodium dichloro cyanurate, fully shake up, after stablizing 2 hours, accurately pipetting 100ml puts in the 250ml iodine flask, add A.R glacial acetic acid 2ml and A.R solid potassium iodide 1g, shake up rearmounted dark place 15 minutes, with 0.0250M sodium thiosulfate standard solution markization, make indicator (get 100ml distilled water simultaneously and do blank test) with the 1%A.R starch solution, be calculated as follows the accurate concentration of chlorine with above-mentioned same operation:
Cl
2（mg/ml）＝ (（A-B）×M×35.45)/(V)
In the formula: A-chlorine standard specimen consumes sodium thiosulfate ml number;
The blank sample of B-consumes sodium thiosulfate ml number;
The volumetric molar concentration mol/L of M-sodium thiosulfate standard solution;
V-standard solutions of chlorine volume (ml);
35.45-the reduction coefficient of chlorine.
Theoretical Calculation: 0.0250mol/L normal sodium thiosulfate solution 1.00ml=886.3 μ g effective chlorine is (with Cl
2Meter).
Chlorine solution after the markization is diluted to 10 μ g/ml to be used for operation.
Add standard chlorine operation liquid and make the series concentration of 0,0.05～1.0mg/L chlorine in the no chlorine water of 100ml volume, each concentration can record the consumption (ml) of corresponding methyl orange operation liquid, sees Table 1:
Three, the present invention surveys the specific operation process of chlorine residue in the water: promptly with the specific purpose tool among the present invention, utilize the methyl orange lean solution to be less than or equal under 2 the condition and survey the process of chlorine residue in the water by structure that can destruction itself behind the oxychlorination takes on a red color and irreversible principle, just:
1, the special-purpose body (Fig. 1) of the present invention being surveyed chlorine residue specific purpose tool in the water is filled with behind the water sample to be measured vertically (the special-purpose body water level mouth (Fig. 1-2) vertically will be positioned at the top of 100ml scale mark), the water sample to be measured that injects will just reach 100ml scale mark place, and then special-purpose body transverse presentation is placed (as Fig. 1).
2, Dropwise 5 drips 1+1AR hydrochloric acid in the water filling gas outlet of special-purpose body (Fig. 1) (Fig. 1-3).
3, get measuring pipette (Fig. 2), mother with left hand, the beaded glass (Fig. 2-1) that food two refers on the compressive belt calibrated pipet, the right hand is arrested ear washing bulb and is aimed at sebific duct (Fig. 2-2) openend that beaded glass (Fig. 2-1) is housed on the calibrated pipet, slowly draw more than the methyl orange operation liquid of 5ml and with liquid level and be adjusted to 0.0ml(Fig. 2-4) locate, then with the long 20 ± 2mm of being with of measuring pipette, the liquid droping port of internal diameter 1 ± 0.2mm sebific duct (Fig. 2-5) oblique cutting is gone in the water level mouth (Fig. 1-2) of special-purpose body (Fig. 1), in light rolling water sample, sebific duct (Fig. 2-2) with finger compressive belt calibrated pipet (Fig. 2) upper glass pearl (Fig. 2-1) bottom, make the methyl orange solution in the suction pipe dropwise splash in the water sample, do not take off to the water sample pinkiness and to end (the loxosis observation water surface), in the water level mouth (Fig. 1-2) of special-purpose body, take out measuring pipette, right-angle view consumes the ml number (read to radix point after) of methyl orange operation liquid, from Figure of description 3, directly find the concentration (mg/L) of chlorine residue the water sample again, or calculate the concentration (mg/L) of chlorine residue by the formula of regression equation y=5.27x+0.15, in the formula: the consumption volume (ml) of y-methyl orange, promptly
x＝ (y-0.15)/5.27 ，（Cl
2mg/L）。
Advantage of the present invention and characteristics:
1, the present invention have soon, accurate, letter, honest and clean advantage:
It is very fast that the present invention surveys a water sample, only needs 1～2 minute, because employing is volumetric method, so its accuracy higher (error ± 0.1～0.2%); Agents useful for same has only two kinds and cheaply general; A complete set of testing tool is also very simple and cheap, and only 15 yuan of its total costs wherein mainly contain one of dedicated pipe (Fig. 1), one of measuring pipette (Fig. 2) and one of little ear washing bulb (and the OT method is wanted 500 yuan at least).
2, instrument be easy to carry (be placed on a handbag in get final product); Reagent long shelf-life and stable (can preserve more than half a year constant at least); Extremely being fit to indoor and outdoor, scene, chlorination station, Rural water supply point, swimming pool etc. locates to use.To sum up, the present invention in all case, and is all available at any time.
3, simple to operate, easy grasp: as long as the operator has the above educational level in junior middle school, learn to grasp in hour, so just help popularizing.
4, this method agents useful for same does not have any pollution, to operator's safety, has thoroughly like this solved the influence that the OT method has carcinogenic factor.
Most preferred embodiment:
This experiment is to use aforesaid specific purpose tool of the present invention: (1) special-purpose body: glass, long 265mm, internal diameter 30mm;
(2) measuring pipette: 0.0～5.0ml, scale be apart from 180mm, and 0.0ml～90 ° corner-centric is apart from 35mm, the long 50mm of silicone tube internal diameter 5mm of big mouth of sheath end, bead D6mm; Be placed in the long 20mm of sebific duct of liquid droping port, internal diameter 1.0mm;
(3) reagent: preparation method as previously mentioned.
(4) concrete steps of Jian Ceing as previously mentioned.
1, our unit's laboratory tap water (storage cistern water, not chlorination) is detected,, consume methyl orange operation liquid 0.1ml, look into Fig. 3, result＜0.05mg/LCl by testing result of the present invention
2, 1.8 minutes detection times.
2, to this city and level road residential dormitory building tap water (near waterworks) test result, consume methyl orange operation liquid 2.0ml, look into Fig. 3, the result is 0.35mg/LCl
2, 1.3 minutes detection times.
Claims (6)
1, " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water " is characterized in that this assay method content comprises:
1. reagent and reagent preparation: the preparation of A methyl orange standard solution;
The preparation of B standard solutions of chlorine and markization.
2. the present invention surveys the specific operation process of chlorine residue in the water: be survey instrument with the specific purpose tool among the present invention promptly, structure and the irreversible principle of utilizing the methyl orange lean solution can destruction itself after pH value is less than or equal under 2 the condition by oxychlorination to take on a red color are surveyed the process of chlorine residue in the water.Be total to two parts.
2, according to the assay method in the claim 1 described " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water ", it is characterized in that (1) reagent and reagent preparation (preparation of A, methyl orange standard solution, the preparation of B standard solutions of chlorine and markization) in this method are meant:
The preparation of A methyl orange standard solution:
Take by weighing 0.100g methyl orange and place the vial of 1L, add a certain amount of hot distilled water dissolving, be cooled to normal temperature then, add 20ml95% again and analyze straight alcohol and be settled to 1L, shake up, this liquid is called stoste.
Get stoste 5.00ml and place the 200ml volumetric flask, add 1+1 and analyze pure hydrochloric acid 0.5ml, with distilled water diluting to 200ml.The above-mentioned solution for preparing should take on a red color, and absorption peak is at 510mm on 721 type spectrophotometers, and the absorbance of 1cm optical path absorption cell is 0.316～0.311, if non-this value of solution, reply stoste is done suitable adjustment.The stoste dilution of adjusting is methyl orange standard operation solution for 1 times.
The preparation of B, standard solutions of chlorine and markization:
(Puritabs is dissolved in the 500ml distilled water accurately to take by weighing the 0.1000g sodium dichloro cyanurate, shake up stablize 2 hours after, accurately pipetting 100ml puts in the 250ml iodine flask, add and analyze pure glacial acetic acid 2ml and analyze pure solid potassium iodide 1g, shake up, put the dark place 15 minutes, with 0.0250M sodium thiosulfate standard solution markization, analyze pure starch solution with 1% and make indicator (get 100ml distilled water simultaneously and do blank test), be calculated as follows the accurate concentration of chlorine with above-mentioned same operation:
Cl
2（mg/ml）＝ (（A-B）×M×35.45)/(V)
In the formula: A-chlorine standard specimen consumes sodium thiosulfate ml number;
The blank sample of B-consumes sodium thiosulfate ml number;
The volumetric molar concentration mol/L of M-sodium thiosulfate standard solution;
35.45-the reduction coefficient of chlorine.
Theoretical Calculation:
0.0250mol/L normal sodium thiosulfate solution 1.00ml=886.3 μ g effective chlorine (with Cl, meter) is diluted to 10 μ g/ml with the chlorine solution after the markization and uses for operation.Add standard chlorine operation liquid and make the series concentration of 0,0.05～1.0 μ g/L chlorine in the no chlorine water of the test volume of 100ml, each concentration can record the consumption (ml) of corresponding methyl orange operation liquid.
3,, it is characterized in that 2. the present invention in this assay method surveys that the specific operation process of chlorine residue refers in the water according to the assay method in the claim 1 described " simple and easy, rapid assay methods of chlorine residue and special specific purpose tool in the water ":
A, the present invention is surveyed the special-purpose body in the chlorine residue specific purpose tool in the water fill with behind the water sample to be measured vertically (the special-purpose body vertically earlier, the water level mouth will be positioned at the top of 100ml scale mark) water sample to be measured that injects will just reach 100ml scale mark place, and then special-purpose body transverse presentation is placed.
B, Dropwise 5 drips 1+1 and analyzes pure hydrochloric acid in the water filling gas outlet of special-purpose body.
C, get measuring pipette, with the mother of left hand, the beaded glasses that food two refers on the compressive belt calibrated pipets, the right hand is arrested ear washing bulb.Aim at the openend that the sebific duct of beaded glass is housed on the measuring pipette, slowly draw more than the methyl orange operation liquid of 5ml and with liquid level and be adjusted to the 0.0ml place, then with the long 20 ± 2mm of being with of measuring pipette, the liquid droping port end of internal diameter 1 ± 0.2mm sebific duct, oblique cutting is gone in the water level mouth special-purpose on the special-purpose body, in light rolling water sample, sebific duct with finger compressive belt calibrated pipet upper glass pearl bottom, make the methyl orange solution in the suction pipe dropwise splash in the water sample, to the water sample pinkiness and till no longer fading, in the water level mouth of special-purpose body, take out measuring pipette then, right-angle view consumes the ml number of methyl orange operation liquid, directly find the concentration (mg/L) of chlorine residue in the water sample again with look-up table, or calculate concentration (the X) (Cl of chlorine residue by the formula of regression equation Y=5.27X+0.15
2Mg/L), the consumption volume (ml) of Y-methyl orange in the formula, that is:
x＝ (y-0.15)/5.27 （Cl
2，mg/L）。
4, the specific purpose tool in " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water " is characterized in that this specific purpose tool comprises:
A, make by colourless uniform glass, sealing two ends, have the 100ml scale mark, one water level mouth is arranged, the garden column " special-purpose body " of a water filling gas outlet (body transverse presentation place and water level mouth above body the time) is arranged on water level mouth right side on 100ml scale mark right side.
B, be with sebific duct at liquid droping port one end, the other end curves 90 ° of bend pipes, and cover is loaded onto the sebific duct of beaded glass and the dropper of 5ml scale is arranged on this bend pipe mouth.
Totally two parts.
5, according to the specific purpose tool in the claim 4 described " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water ", it is characterized in that the two ends that the special-purpose body in this specific purpose tool seals are smooth, long 260 ± the 10mm of body, internal diameter 32 ± 2mm, water level mouth and water filling gas outlet on the body are high 4-5mm, the short cylindrical shape mouth of internal diameter 4-5mm, two mouthfuls centre distance is 15 ± 2mm.
6, according to the specific purpose tool in the claim 4 described " simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water ", it is characterized in that the measuring pipette in this specific purpose tool is a 5ml calibrated pipet.The scale mark characteristics of this suction pipe are that the scale with distance suction pipe liquid droping port (thin end) farthest is decided to be the 0ml scale mark, curve 90 ° from the 0ml scale mark to not being with the scale mark direction to extend to apart from 0ml scale mark 30 ± 5mm, and make the external diameter of pipe remain on 6-7mm, be 35 ± 5mm by 90 ° of pipe bent position to the suction pipe end; Suction pipe terminal with the D=6mm beaded glass is housed, long 50 ± 5mm, the sebific duct of internal diameter 5mm (silica gel or latex) combination; Liquid droping port one end (thin end) at suction pipe is with long 20 ± 2mm, the sebific duct of internal diameter 1mm (silica gel or latex).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106462 CN1067739A (en) | 1992-04-07 | 1992-04-07 | Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106462 CN1067739A (en) | 1992-04-07 | 1992-04-07 | Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water |
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| Publication Number | Publication Date |
|---|---|
| CN1067739A true CN1067739A (en) | 1993-01-06 |
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ID=4942133
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|---|---|---|---|
| CN 92106462 Pending CN1067739A (en) | 1992-04-07 | 1992-04-07 | Simple and easy, rapid assay methods of chlorine residue and specific purpose tool in the water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636484A (en) * | 2012-05-09 | 2012-08-15 | 河北省电力研究院 | Method for quickly testing presence of oxide in hydrochloric acid |
| CN104781653A (en) * | 2012-11-06 | 2015-07-15 | 栗田工业株式会社 | Method for automatically measuring concentration of dissolved substance |
| CN105445265A (en) * | 2015-12-03 | 2016-03-30 | 上海仪电科学仪器股份有限公司 | Method for preparing permanent residual chlorine standard colorimetric serial solution |
| CN107037177A (en) * | 2016-02-03 | 2017-08-11 | 中国科学院大连化学物理研究所 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
-
1992
- 1992-04-07 CN CN 92106462 patent/CN1067739A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636484A (en) * | 2012-05-09 | 2012-08-15 | 河北省电力研究院 | Method for quickly testing presence of oxide in hydrochloric acid |
| CN104781653A (en) * | 2012-11-06 | 2015-07-15 | 栗田工业株式会社 | Method for automatically measuring concentration of dissolved substance |
| CN104781653B (en) * | 2012-11-06 | 2016-08-17 | 栗田工业株式会社 | The automatic measuring method of dissolved matter concentration |
| CN104781653B9 (en) * | 2012-11-06 | 2016-11-09 | 栗田工业株式会社 | The automatic measuring method of solute concentration |
| CN105445265A (en) * | 2015-12-03 | 2016-03-30 | 上海仪电科学仪器股份有限公司 | Method for preparing permanent residual chlorine standard colorimetric serial solution |
| CN105445265B (en) * | 2015-12-03 | 2018-06-29 | 上海仪电科学仪器股份有限公司 | The preparation method of permanent chlorine residue standard colorimetric serial solution |
| CN107037177A (en) * | 2016-02-03 | 2017-08-11 | 中国科学院大连化学物理研究所 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
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