CN102095724B - Method for determining copper content in water by biquinolyl spectrophotometry - Google Patents
Method for determining copper content in water by biquinolyl spectrophotometry Download PDFInfo
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Abstract
The invention relates to a method for determining copper content in water by biquinolyl spectrophotometry, which is convenient in operation and has the advantages of short time and high accuracy. The method comprises the following steps: (1) preparing a copper standard solution; (2) sampling; (3) detecting the samples: (i) calibrating; (ii) testing; (iii) conducting blank test: and (iv) conducting a calibration test.; and (4) displaying the result: searching the data from the calibration curve as the copper concentration in the water sample.
Description
Technical field
The invention belongs to the detection method field of water quality copper, the detection diquinoline AAS of the water quality copper that especially a kind of minute is short, easy and simple to handle and accuracy is high.
Background technology
The detection method of tradition water quality copper has the detection 2 of water quality copper, 9-dimethyl-1, the detection sodium diethyldithiocarbamate AAS of 10-ferrosin AAS and water quality copper.These two kinds of methods have all been used the step of extraction, make the mensuration process complicated, and the time spent is longer, and are not suitable for this prescription of instrument production use.
Summary of the invention
The detection diquinoline AAS that the purpose of this invention is to provide the water quality copper that a kind of minute is short, easy and simple to handle and accuracy is high.
Technical scheme of the present invention is: the detection diquinoline AAS of water quality copper is characterized in that comprising the following steps:
(1) makes the copper standard reserving solution: take by weighing the electrolysis copper wire or the Copper Foil of 0.0999-0.10001g polishing, place conical flask, add 10mL water and 5mL nitric acid (ρ
20=1.40g/mL), heating is all dissolved copper, boils solution to drive away nitrogen oxides, and solution cooling back adds 50mL water, quantitatively transfers in the 1000mL volumetric flask, is diluted with water to graticule and mixing;
(2) sampling and sample: gather 1000mL water sample to be measured, from water sample, get two parts of even samples, every part of 100mL places beaker, as clearing up sample;
(3) detect, specifically comprise the following steps:
1. calibration: with seven volumetric flasks, add the copper standard solution 10mL of 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L, 5.00mg/L, 6.00mg/L, 7.00mg/L respectively, in volumetric flask, add ρ respectively
20=1.84g/mL sulfuric acid 1mL fully shakes up; Then, add Ammonia, be transferred to 2.9-3.1 to pH value according to give in the volumetric flask respectively by the addition of 1mL at every turn;
Give respectively to add buffer solution 2.8-3.2mL in the volumetric flask, and then add reductive agent 0.9-1.1mL, fully shake up the back and add diquinoline 0.9-1.1mL, produce the aubergine complex compound;
Reacted solution is put into the 10mm cuvette respectively, and sentencing water at 560nm is reference, measures the absorbance of examination part respectively;
Do reference with water, from the absorbance that records the copper standard solution, deduct after the reagent blank absorbance and draw calibration curve with corresponding copper content; If the content of copper is lower than 1mg/L in the examination part, it is lower also need to draw a concentration series, is the calibration curve of the 9.5-10.5% of original concentration; Draw copper standard solution 0.1-1.0mg/L, operate, when measuring absorbance, use the 30mm cuvette instead by above-mentioned steps;
2. measure, specifically comprise the following steps:
(A) clear up: in every part of sample, add ρ respectively
20Sulfuric acid 1mL and the ρ of=1.84g/mL
20=1.40g/mL nitric acid 5mL, putting into every weight then is the beaded glass 4-5 grain of 0.3-0.5g, puts on the electric hot plate heating and clears up till emit the white cigarette of sulfuric anhydride; If solution still is with look, the cooling back adds ρ
20=1.40g/mL nitric acid 5mL continues to be heated to and emits the white cigarette of sulfuric anhydride, and is colourless up to solution;
Solution cooling back adds 70-90mL water, is heated to boiling and keeps 3 minutes, and the filter of cooling back is gone in the volumetric flask, adds to graticule and mixing with washings;
First part of sample in step (2) sampling and the sample operated by following step (B);
(B) measure: the sample after will clearing up is got 10mL, places volumetric flask, and 1. middle set by step method begins to measure from the hydro-oxidation ammonium;
After measuring the absorbance of examination part, deduct blank absorbency after, check in the content of copper from calibration curve;
3. blank assay: replace sample with 100mL water, handle by (A) step and (B) step, blank sample is measured under the same conditions simultaneously;
4. calibration test: second part in step (2) sampling and the sample cleared up draw part solution in the sample, add copper standard solution number milliliter, make examination part volume be no more than 10mL; Measure by (B) step; Repeat operation, more than three times, to define noiseless influence;
(4) result representes step: the data that check in from calibration curve are the concentration of copper the water sample.
Effect of the present invention is: the minimum detectability that this method is measured copper is 0.1mg/L, and the upper limit can arrive 7mg/L, and can only arrive 3mg/L and 0.60mg/L for detecting the upper limit with the most close two sets of plan of this programme.This method can be measured the copper content that is higher than in the water quality that other two kinds of methods detect the upper limit, avoids diluting the error of bringing.
Below in conjunction with not limiting embodiment the present invention is done further explanation.
Embodiment
Embodiment 1:
The detection diquinoline AAS of water quality copper comprises the following steps:
1, the scope of application
(1) this detection method is applicable to the mensuration of laboratory for copper in the day water, sanitary sewage and the industrial waste water; (2) this detection method is applicable to the mensuration of online automatic detection instrument for copper in the day water, sanitary sewage and the industrial waste water.
The cuvette light path is 10mm, and the minimum detectability of copper is 0.1mg/L, is limited on the mensuration: 7mg/L.
2, definition: (1) soluble copper: without the water sample of acidifying, through the copper concentration that records behind the 0.45um filter membrane; (2) total copper: the water sample of filtered, the copper concentration that after acutely clearing up, records.
3, principle.Be reduced to cuprous ion to bivalent cupric ion with oxammonium hydrochloride, in slightly acidic solution, cuprous ion and diquinoline reaction generate the aubergine complex compound, measure absorbance at wavelength 560nm place.
4, reagent.
In the mensuration process, the double distilled water that all uses deionized water or full glass distiller to make.Except as otherwise noted, all use the AR of generally acknowledging.
(4.1) sulfuric acid (H
2SO
4): ρ
20=1.84g/mL, top grade is pure;
(4.2) nitric acid (HNO
3): ρ
20=1.40g/mL, top grade is pure;
(4.3) hydrochloric acid (HCl): ρ
20=1.19g/mL;
(4.4) reductive agent;
(4.5) Ammonia;
(4.6) buffer solution
(4.7) developer: diquinoline solution
(4.8) copper standard reserving solution: 100mg/L
Take by weighing the electrolysis copper wire or the Copper Foil (purity is more than 99.9%) of 0.1000 ± 0.0001g polishing, place the 250mL conical flask, add 10mL water and 5mL nitric acid (4.2), when reaction rate is slack-off, heat slightly, make whole copper dissolutions.Then, boil solution to drive away nitrogen oxides.The cooling back adds 50mL water, quantitatively transfers in the 1000mL volumetric flask, is diluted with water to graticule and mixing.
The solution that is diluted to desired concn in use is in order to measuring.
5, instrument.Common experimental chamber equipment: (1) spectrophotometer, (2) conical flask, volumetric flask 25mL.
6, sampling and sample
(6.1) laboratory sample.Gather the 1000mL water sample, measure immediately,, be adsorbed on the sampling container wall, in every liter of sample, add the hydrochloric acid of 5mL (1+1), be acidified to PH and be about the 1.5. sampling container and should use Plastic Drum in order to prevent copper ion if can not measure immediately.
(6.2) sample.From water sample, get two parts of even samples, every part of 100mL places the 250mL beaker, as clearing up sample.
7, step
(7.1) calibration.
With seven volumetric flasks, add 1.00,2.00,3.00,4.00,5.00,6.00 respectively, the copper standard solution 10mL of 7.00mg/L, add 1mL sulfuric acid (ρ
20=1.84g/mL), fully shake up.Each addition of pressing 1mL adds Ammonia, is transferred to 3 to pH value.
Add buffer solution (4.6) 3mL, add reductive agent (4.4) 1mL again, fully shake up the back and add developer diquinoline 1mL, produce the aubergine complex compound.
Reacted solution is put into the 10mm cuvette, and sentencing water at 560nm is reference, measures the absorbance of examination part.
Do reference with water, from the absorbance that records the copper standard solution, deduct after the reagent blank absorbance and draw calibration curve with corresponding copper content.
If the content of copper is lower than 1mg/L in the examination part, also need draw a calibration curve that concentration series is lower, be 10% calibration curve of original concentration.Draw copper standard solution 0.1-1.0mg/L, operate by above-mentioned steps.When measuring absorbance, use the 30mm cuvette instead.
(7.2) measure
(7.2.1) clear up.In every part of sample, add 1mL sulfuric acid (ρ
20=1.84g/mL) with 5mL nitric acid (ρ
20=1.40g/mL), and put into the beaded glass 4-5 grain that every weight is 0.3-0.5g, put on the electric hot plate heating and clear up (noting not splash) till emit the white cigarette of sulfuric anhydride.If solution still is with look, the cooling back adds 5mL nitric acid, continues to be heated to and emits till the white cigarette of sulfuric anhydride.Repeat aforesaid operations in case of necessity, colourless up to solution.
The cooling back adds about 80mL water, is heated to boiling and keeps 3min, and the filter of cooling back is gone in the 100mL volumetric flask, with water washing beaker and filter paper, adds to graticule and mixing with washings.
Sample (D) after second part cleared up is preserved, and is used for test revision (7.4).Operate first part of sample by following step.
(7.2.2) measure.Sample after will clearing up is got 10mL, places volumetric flask, and the step of pressing (7.1) begins to measure from the hydro-oxidation ammonium.
After measuring the absorbance of examination part, deduct blank absorbency after, check in the content of copper from calibration curve.
(7.3) blank assay
Replace sample with 100mL water, by (7.2.1) and (7.2.2) step handle.Blank sample is measured under the same conditions simultaneously.
(7.4) calibration test
Clear up the sample (D) solution of drawing an amount of volume from second part, add copper standard solution number milliliter, make an examination part volume be no more than 10mL, measure by 7.2.2, repeat operation, the number of times of repetitive operation is greater than three times, to define noiseless influence.
8, the result representes
From calibration curve look into the concentration that is copper the water sample.
Embodiment 2: the detection diquinoline AAS of water quality copper is characterized in that comprising the following steps:
(1) makes the copper standard reserving solution: take by weighing the electrolysis copper wire or the Copper Foil of 0.0999-0.10001g polishing, place conical flask, add 10mL water and ρ
20=1.40g/mL nitric acid 5mL nitric acid, heating is all dissolved copper, boils solution to drive away nitrogen oxides, and solution cooling back adds 50mL water, quantitatively transfers in the 1000mL volumetric flask, is diluted with water to graticule and mixing;
(2) sampling and sample: gather 1000mL water sample to be measured, from water sample, get two parts of even samples, every part of 100mL places beaker, as clearing up sample;
(3) detect, specifically comprise the following steps:
1. calibration: with seven volumetric flasks, add the copper standard solution 10mL of 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L, 5.00mg/L, 6.00mg/L, 7.00mg/L respectively, in volumetric flask, add ρ respectively
20=1.84g/mL sulfuric acid 1mL fully shakes up; Then, add Ammonia, be transferred to 2.9 to pH value according to give in the volumetric flask respectively by the addition of 1mL at every turn;
Give respectively to add buffer solution 2.8mL in the volumetric flask, and then add reductive agent 0.9mL, fully shake up the back and add diquinoline 0.9mL, produce the aubergine complex compound;
Reacted solution is put into the 10mm cuvette respectively, and sentencing water at 560nm is reference, measures the absorbance of examination part respectively;
Do reference with water, from the absorbance that records the copper standard solution, deduct after the reagent blank absorbance and draw calibration curve with corresponding copper content; If the content of copper is lower than 1mg/L in the examination part, it is lower also need to draw a concentration series, is 9.5% calibration curve of original concentration; Draw copper standard solution 0.1-1.0mg/L, operate, when measuring absorbance, use the 30mm cuvette instead by above-mentioned steps;
2. measure, specifically comprise the following steps:
(A) clear up: in every part of sample, add ρ respectively
20Sulfuric acid 1mL and the ρ of=1.84g/mL
20=1.40g/mL nitric acid 5mL, putting into every weight then is the beaded glass 4-5 grain of 0.3-0.5g, puts on the electric hot plate heating and clears up till emit the white cigarette of sulfuric anhydride; If solution still is with look, the cooling back adds ρ
20=1.40g/mL nitric acid 5mL continues to be heated to and emits the white cigarette of sulfuric anhydride, and is colourless up to solution;
Solution cooling back adds 70-90mL water, is heated to boiling and keeps 3 minutes, and the filter of cooling back is gone in the volumetric flask, adds to graticule and mixing with washings;
First part of sample in step (2) sampling and the sample operated by following step (B);
(B) measure: the sample after will clearing up is got 10mL, places volumetric flask, and 1. middle set by step method begins to measure from the hydro-oxidation ammonium;
After measuring the absorbance of examination part, deduct blank absorbency after, check in the content of copper from calibration curve;
3. blank assay: replace sample with 100mL water, handle by (A) step and (B) step, blank sample is measured under the same conditions simultaneously;
4. calibration test: second part in step (2) sampling and the sample cleared up draw part solution in the sample, add copper standard solution number milliliter, make examination part volume be no more than 10mL; Measure by (B) step; Repeat operation, more than three times, to define noiseless influence;
(4) result representes step: the data that check in from calibration curve are the concentration of copper the water sample.
Embodiment 3: the detection diquinoline AAS of water quality copper is characterized in that comprising the following steps:
(1) makes the copper standard reserving solution: take by weighing the electrolysis copper wire or the Copper Foil of 0.0999-0.10001g polishing, place conical flask, add 10mL water and ρ
20=1.40g/mL nitric acid 5mL nitric acid, heating is all dissolved copper, boils solution to drive away nitrogen oxides, and the solution cooling adds 50mL water after the solution cooling, quantitatively transfers in the 1000mL volumetric flask, is diluted with water to graticule and mixing;
(2) sampling and sample: gather 1000mL water sample to be measured, from water sample, get two parts of even samples, every part of 100mL places beaker, as clearing up sample;
(3) detect, specifically comprise the following steps:
1. calibration: with seven volumetric flasks, add the copper standard solution 10mL of 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L, 5.00mg/L, 6.00mg/L, 7.00mg/L respectively, in volumetric flask, add ρ respectively
20=1.84g/mL sulfuric acid 1mL fully shakes up; Then, add Ammonia, be transferred to 3.1 to pH value according to give in the volumetric flask respectively by the addition of 1mL at every turn;
Give respectively to add buffer solution 3.2mL in the volumetric flask, and then add reductive agent 1.1mL, fully shake up the back and add diquinoline 1.1mL, produce the aubergine complex compound;
Reacted solution is put into the 10mm cuvette respectively, and sentencing water at 560nm is reference, measures the absorbance of examination part respectively;
Do reference with water, from the absorbance that records the copper standard solution, deduct after the reagent blank absorbance and draw calibration curve with corresponding copper content; If the content of copper is lower than 1mg/L in the examination part, it is lower also need to draw a concentration series, is 9.5% calibration curve of original concentration; Draw copper standard solution 0.1-1.0mg/L, operate, when measuring absorbance, use the 30mm cuvette instead by above-mentioned steps;
2. measure, specifically comprise the following steps:
(A) clear up: in every part of sample, add ρ respectively
20Sulfuric acid 1mL and the ρ of=1.84g/mL
20=1.40g/mL nitric acid 5mL, putting into every weight then is the beaded glass 4-5 grain of 0.3-0.5g, puts on the electric hot plate heating and clears up till emit the white cigarette of sulfuric anhydride; If solution still is with look, the cooling back adds ρ
20=1.40g/mL nitric acid 5mL continues to be heated to and emits the white cigarette of sulfuric anhydride, and is colourless up to solution;
Solution cooling back adds 70-90mL water, is heated to boiling and keeps 3 minutes, and the filter of cooling back is gone in the volumetric flask, adds to graticule and mixing with washings;
First part of sample in step (2) sampling and the sample operated by following step (B);
(B) measure: the sample after will clearing up is got 10mL, places volumetric flask, and 1. middle set by step method begins to measure from the hydro-oxidation ammonium;
After measuring the absorbance of examination part, deduct blank absorbency after, check in the content of copper from calibration curve;
3. blank assay: replace sample with 100mL water, handle by (A) step and (B) step, blank sample is measured under the same conditions simultaneously;
4. calibration test: second part in step (2) sampling and the sample cleared up draw part solution in the sample, add copper standard solution number milliliter, make examination part volume be no more than 10mL; Measure by (B) step; Repeat operation, more than three times, to define noiseless influence;
(4) result representes step: the data that check in from calibration curve are the concentration of copper the water sample.
Claims (1)
1. the detection diquinoline AAS of water quality copper is characterized in that comprising the following steps:
(1) makes the copper standard reserving solution: take by weighing the electrolysis copper wire or the Copper Foil of 0.0999-0.10001g polishing, place conical flask, add 10mL water and 5mL ρ
20The nitric acid heating of=1.40g/mL is all dissolved copper, boils solution to drive away nitrogen oxides, and solution cooling back adds 50mL water, quantitatively transfers in the 1000mL volumetric flask, is diluted with water to graticule and mixing;
(2) sampling and sample: gather 1000mL water sample to be measured, from water sample, get two parts of even samples, every part of 100mL places beaker, as clearing up sample;
(3) detect, specifically comprise the following steps:
1. calibration: with seven volumetric flasks, add the copper standard solution 10mL of 1.00mg/L, 2.00mg/L, 3.00mg/L, 4.00mg/L, 5.00mg/L, 6.00mg/L, 7.00mg/L respectively, in volumetric flask, add ρ respectively
20=1.84g/mL sulfuric acid 1mL fully shakes up; Then, add Ammonia, be transferred to 2.9-3.1 to pH value according to give in the volumetric flask respectively by the addition of 1mL at every turn;
Give respectively to add buffer solution 2.8-3.2mL in the volumetric flask, and then add reductive agent 0.9-1.1mL, fully shake up the back and add diquinoline 0.9-1.1mL, produce the aubergine complex compound;
Reacted solution is put into the 10mm cuvette respectively, and sentencing water at 560nm is reference, measures the absorbance of sample respectively;
Do reference with water, from the absorbance that records the copper standard solution, deduct after the reagent blank absorbance and draw calibration curve with corresponding copper content; If the content of copper is lower than 1mg/L in the sample, it is lower also need to draw a concentration series, is the calibration curve of the 9.5-10.5% of original concentration; Draw copper standard solution 0.1-1.0mg/L, operate, when measuring absorbance, use the 30mm cuvette instead by above-mentioned steps;
2. measure, specifically comprise the following steps:
(A) clear up: in every part of sample, add ρ respectively
20Sulfuric acid 1mL and the ρ of=1.84g/mL
20=1.40g/mL nitric acid 5mL, putting into every weight then is the beaded glass 4-5 grain of 0.3-0.5g, puts on the electric hot plate heating and clears up till emit the white cigarette of sulfuric anhydride; If solution still is with look, the cooling back adds ρ
20=1.40g/mL nitric acid 5mL continues to be heated to and emits the white cigarette of sulfuric anhydride, and is colourless up to solution;
Solution cooling back adds 70-90mL water, is heated to boiling and keeps 3 minutes, and the filter of cooling back is gone in the volumetric flask, adds to graticule and mixing with washings;
First part of sample in step (2) sampling and the sample operated by following step (B);
(B) measure: the sample after will clearing up is got 10mL, places volumetric flask, and 1. middle set by step method begins to measure from the hydro-oxidation ammonium;
After measuring the absorbance of sample, deduct blank absorbency after, check in the content of copper from calibration curve;
3. blank assay: replace sample with 100mL water, handle by (A) step and (B) step, blank sample is measured under the same conditions simultaneously;
4. calibration test: second part in step (2) sampling and the sample cleared up draw part solution in the sample, adding copper standard solution number milliliter makes volume of sample be no more than 10mL; Measure by (B) step; Repeat operation, more than three times, to define noiseless influence;
(4) result representes step: the data that check in from calibration curve are the concentration of copper the water sample.
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| CN102252986B (en) * | 2011-06-16 | 2013-08-21 | 河南工业大学 | Kit for detecting beta-lactamase in raw milk and dairy products and detection method thereof |
| CN102928353B (en) * | 2012-10-24 | 2014-10-22 | 同济大学 | Preparation method and using method for developing detection piece for determining copper ions in water |
| CN105277540B (en) * | 2015-02-05 | 2018-03-23 | 温州医科大学 | Copper ion field fast detection method in a kind of water for eliminating reagent blank influence |
| CN105527235B (en) * | 2015-12-30 | 2018-04-17 | 汕头大学医学院 | A kind of method of liquid-liquid extraction GFAAS methods measure monovalence copper content |
| WO2019056289A1 (en) * | 2017-09-22 | 2019-03-28 | 万宝矿产有限公司 | Method for determining acid-soluble copper in copper ore |
| CN107764817A (en) * | 2017-10-18 | 2018-03-06 | 苏州泰坤检测技术有限公司 | The online test method of content of beary metal in a kind of water quality |
| CN108414467A (en) * | 2018-05-25 | 2018-08-17 | 中科广化（重庆）新材料研究院有限公司 | The ultraviolet specrophotometer assay method of sodium dimethyl dithiocarbamate content in a kind of solution |
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| WO2005032693A2 (en) * | 2003-08-29 | 2005-04-14 | Velocys Inc. | Process for separating nitrogen from methane using microchannel process technology |
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Owner name: QINGDAO JIAMING MEASUREMENT AND CONTROL TECHNOLOGY Free format text: FORMER NAME: QINGDAO JIAMING MEASURING AND CONTROL INSTRUMENT CO., LTD. |
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Address after: 266000 Shandong city of Qingdao province Fuzhou Northroad 169-919 Patentee after: QINGDAO JIAMING MEASUREMENT AND CONTROL TECHNOLOGY CO., LTD. Address before: 266000 Shandong city of Qingdao province Fuzhou Northroad 169-919 Patentee before: Qingdao Jiaming Measurement and Control Instrument Co., Ltd. |