CN102262063A - Method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry - Google Patents

Method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry Download PDF

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CN102262063A
CN102262063A CN201110174453A CN201110174453A CN102262063A CN 102262063 A CN102262063 A CN 102262063A CN 201110174453 A CN201110174453 A CN 201110174453A CN 201110174453 A CN201110174453 A CN 201110174453A CN 102262063 A CN102262063 A CN 102262063A
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prussiate
water
isonicotinic acid
spectrophotometry
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吴佑琼
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Abstract

The invention discloses a method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry. Under the condition that chloramine T exists in a weak acid medium, the prussiate and isonicotinic acid-thiobarbituric acid form red-blue dye which has a principle of dual absorption peaks; a novel method for measuring the trace quantity of prussiate in water through experiment, namely the isonicotinic acid-thiobarbituric acid dual-wavelength superposition spectrophotometry is established and provides a simple, convenient and sensitive analyzing method for measuring the trace quantity of prussiate in a water sample; and meanwhile, the application range of thiobarbituric acid is widened.

Description

The method of micro cyanide in the dual wavelength stack spectrophotometry water
Technical field
The present invention relates to a kind of method of measuring micro cyanide in the water.
Background technology
Generally do not contain prussiate (CN in the natural water -), it is mainly derived from industrial pollution prussiate, and prussiate combines with cytochrome oxidase after entering human body, makes the people rapidly dead because of anoxic, so prussiate is as one of toxicologic index of water quality monitoring.Limiting the quantity of of regulation prussiate is respectively 0.20 mg/L and 0.05 mg/L in water environment quality standard (III class) and drinking water sanitary standard.The assay method national standard of micro cyanide is recommended in surface water and the Drinking Water mainly contains isonicotinic acid-pyrazolone photometry, isonicotinic acid-barbiturates photometry and pyridine-barbiturates photometry, but does not see bibliographical information as yet with isonicotinic acid-thiobarbituricacid dual wavelength micro cyanide that superposes in the spectrphotometric method for measuring water.
Summary of the invention
The objective of the invention is to provide a kind of energy repeatability and good stability, with the method for micro cyanide in isonicotinic acid-thiobarbituricacid dual wavelength stack spectrphotometric method for measuring water.
The object of the present invention is achieved like this: the method for micro cyanide in a kind of dual wavelength stack spectrophotometry water,
(1) gets prussiate standard solution 0～5.0 mL respectively in a plurality of 10 mL color comparison tubes, NaOH solution to 5 mL that adds 0.05 mol/L, the adding phenolphthalein indicator transfers to redness with acetic acid solution and just disappears, add buffer solution 2.0 mL, toluene-sodium-sulfonchloramide solution 0.20 mL mixing, place 4 min, add isonicotinic acid-thiobarbituricacid solution 2.0 mL and add pure water to scale 10mL mixing, with the reagent blank is reference, measures the maximum absorbance A of each pipe at 2～4 min in 525 nm places with 2 cm cuvettes λ 1, continue to be placed to 35 min, measure the absorbance A of respectively managing 642 nm places with method λ 2, calculate Δ A=A λ 1+ A λ 2, with CN -Content is to Δ A drawing standard curve;
(2) getting 250 mL contains the prussiate water sample and distills, NaOH solution with 5.0 mL, 0.50 mol/L is made absorption liquid, collect distillate to 50.0 mL, get 5.0 mL (1) time-and-motion study absorbance Δ A set by step each the branch, it is quantitative to carry out prussiate with calibration curve method, and carry out method contrast with isonicotinic acid-barbiturates photometry, do the mark-on recovery test simultaneously;
(3) under the experiment condition of step (2), CN -Form red-blue dyes with isonicotinic acid-thiobarbituricacid, by UV spectrophotometer measuring, this dyestuff respectively has an absorption peak at 520～530 nm and 642nm respectively, can judge and contain oxide in the water sample.
The prussiate concentration of standard solution is 0.10 mg/mL.
Buffer solution in the step (1) is potassium dihydrogen phosphate or the sodium hydroxide buffer solution of concentration 0.05 mol/L, pH value 5.8.
The preparation process of the isonicotinic acid in the step (1)-thiobarbituricacid solution is to take by weighing NaOH solution 28～30 mL that 2.0 g thiobarbituricacids and 2.5 g isonicotinic acid add 1.0 mol/L, stirs to make its dissolving back be settled to 100 mL with pure water.
Step (1) toluene-sodium-sulfonchloramide solution concentration is 10.0 g/L.
The method of micro cyanide in the dual wavelength stack spectrophotometry water provided by the invention, utilization is in weak acidic medium and under the toluene-sodium-sulfonchloramide existence condition, prussiate and isonicotinic acid-thiobarbituricacid form a red-blue dyes, this dyestuff respectively has an absorption peak at 525 nm and 642 nm respectively, and its absorbance A λ 1And A λ 2And sum of the two Δ A all is the characteristic of good linear relationship in certain scope with cyanide content, set up a kind of new method-isonicotinic acid-thiobarbituricacid dual wavelength stack photometry of measuring micro cyanide in the water through experiment on this basis.This method cyanide content is at 0～4.0 μ g/(10.0 mL) meet law of Beer in the scope, method is used for the mensuration of water sample micro cyanide, its result and national standard method match, and recovery of standard addition is 96%～104%, the selectivity of method, stable satisfactory.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples.
Fig. 1 is an abosrption spectrogram of the present invention, and curve 1 is reagent blank (to a water) among the figure; Curve 2 is CN -Color development system (to water); Curve 3 is CN -Color development system (to reagent blank).
Fig. 2 is system stability test figure of the present invention, and curve 1 is CN among the figure -With the absorbance of isonicotinic acid-thiobarbituricacid at 525 nm places; Curve 2CN -With the absorbance of isonicotinic acid-thiobarbituricacid at the 642nm place.
Embodiment
Embodiment:
One, key instrument and reagent:
Ultraviolet-visible pectrophotometer: TU-1810SPC type, the general all purpose instrument company limited of analysing in Beijing;
The prussiate standard solution: the accurate concentration of 0.10 mg/mL(is demarcated with silver salt method), face the time spent to be diluted to 1.0 μ g/mL with the NaOH of 0.05 mol/L; 0.05 potassium dihydrogen phosphate/sodium hydroxide buffer solution of mol/L: pH 5.8;
Isonicotinic acid-thiobarbituricacid solution: take by weighing NaOH solution 28～30 mL that 2.0 g thiobarbituricacids and 2.5 g isonicotinic acid add 1.0 mol/L, it is nearly neutrality that stirring makes its dissolving back be settled to this pH value of solution of 100 mL(with pure water);
Toluene-sodium-sulfonchloramide solution: 10.0 g/L, face the time spent preparation;
NaOH solution; 0.50,0.05 mol/L;
Acetic acid solution (3+97);
1.0 the phenolphthalein indicator of g/L;
Above reagent is pure for analyzing, and experimental water is ultrapure water (18.25 Μ Ω cm).
Two, determination step:
(1) gets prussiate standard solution 0～5.0 mL respectively in a plurality of 10 mL color comparison tubes, NaOH solution to 5 mL that adds 0.05 mol/L, the adding phenolphthalein indicator transfers to redness with acetic acid solution and just disappears, add buffer solution 2.0 mL, toluene-sodium-sulfonchloramide solution 0.20 mL mixing, place 4 min, add isonicotinic acid-thiobarbituricacid solution 2.0 mL and add pure water to scale 10mL mixing, with the reagent blank is reference, measures the maximum absorbance A of each pipe at 2～4 min in 525 nm places with 2 cm cuvettes λ 1, continue to be placed to 35 min, measure the absorbance A of respectively managing 642 nm places with method λ 2, calculate Δ A=A λ 1+ A λ 2, with CN -Content is to Δ A drawing standard curve;
(2) getting 250 mL contains the prussiate water sample and distills, NaOH solution with 5.0 mL, 0.50 mol/L is made absorption liquid, collect distillate to 50.0 mL, get 5.0 mL (1) time-and-motion study absorbance Δ A set by step each the branch, it is quantitative to carry out prussiate with calibration curve method, and carry out method contrast with isonicotinic acid-barbiturates photometry, do the mark-on recovery test simultaneously;
(3) under the experiment condition of step (2), CN -Form red-blue dyes with isonicotinic acid-thiobarbituricacid, by UV spectrophotometer measuring, this dyestuff respectively has an absorption peak at 520～530 nm and 642nm respectively, can judge and contain oxide in the water sample.
Three, test result analysis:
The influence of coexisting substances
As the CN that measures 0.20mg/L -, relative error allows following material (in mg/L) coexistence: phenol (10) in ± 5% scope; Cl -, SO 4 -2, NO 3 -, F -, NH 4 +(20); NO 2 -, S -2(5), the selectivity of visual method is good.
2.6 standard regression curve
CN -Content meets law of Beer in 0～0.40 μ g/mL scope, the regression equation of typical curve and the apparent molar absorption coefficient of being tried to achieve by the rate of curve method are respectively: Δ A=3.547C (CN-, ug/mL)-0.0029, r=0.9996, ε=4.61 * 10 4L/ (molcm)
If in Δ A=0.02, its concentration limit 0.003 μ g/mL.
Colour stability
Experiment shows, CN -At first form orchil with isonicotinic acid-thiobarbituricacid, become blueness then gradually, it is at the absorbance (A at 525 nm places λ 1, Fig. 2 curve 1) before this fast rise reach stable maximal value, very fast then decline, and at the absorbance (A at 642 nm places λ 2, Fig. 2 curve 2) and the speed that rises and descend is all slower, but the room temperature lower body ties up to 525 nm and 642 nm absorbances are basicly stable at 2～4 min and 35～50 min respectively, sees Fig. 2.
Repeated experiment
With this law to 0.50 μ g and 2.00 μ gCN -Titer and the replicate determination of 2 portions of water sample distillates 5 times, its measured value are respectively 0.51 μ g and 2.00 μ g, 48.4 μ g/L and 22.2 μ g/L, and relative standard deviation (RSD) is respectively 1.8% and 1.1%, 2.0% and 3.5%, and the repeatability of method is good.
The water sample analysis result
Get 5 parts of water samples by the method time-and-motion study cyanide content that Ben Mingfa provides, use isonicotinic acid-barbiturates photometry simultaneously [5]Carry out the method contrast, and do the mark-on recovery test.The result shows that this law and National Standard Method measurement result match, and recovery of standard addition is 96%～104%, the results are shown in Table 1.
Table 1 sample analysis result
Figure 810436DEST_PATH_IMAGE002

Claims (5)

1. the method for micro cyanide in the dual wavelength stack spectrophotometry water is characterized in that:
(1) gets prussiate standard solution 0～5.0 mL respectively in a plurality of 10 mL color comparison tubes, NaOH solution to 5 mL that adds 0.05 mol/L, the adding phenolphthalein indicator transfers to redness with acetic acid solution and just disappears, add buffer solution 2.0 mL, toluene-sodium-sulfonchloramide solution 0.20 mL mixing, place 4 min, add isonicotinic acid-thiobarbituricacid solution 2.0 mL and add pure water to scale 10mL mixing, with the reagent blank is reference, measures the maximum absorbance A of each pipe at 2～4 min in 525 nm places with 2 cm cuvettes λ 1, continue to be placed to 35 min, measure the absorbance A of respectively managing 642 nm places with method λ 2, calculate Δ A=A λ 1+ A λ 2, with CN -Content is to Δ A drawing standard curve;
(2) getting 250 mL contains the prussiate water sample and distills, NaOH solution with 5.0 mL, 0.50 mol/L is made absorption liquid, collect distillate to 50.0 mL, get 5.0 mL (1) time-and-motion study absorbance Δ A set by step each the branch, it is quantitative to carry out prussiate with calibration curve method, and carry out method contrast with isonicotinic acid-barbiturates photometry, do the mark-on recovery test simultaneously;
(3) under the experiment condition of step (2), CN -Form red-blue dyes with isonicotinic acid-thiobarbituricacid, by UV spectrophotometer measuring, this dyestuff respectively has an absorption peak at 520～530 nm and 642nm respectively, can judge and contain oxide in the water sample.
2. the method for micro cyanide in the dual wavelength stack spectrophotometry water according to claim 1, it is characterized in that: the prussiate concentration of standard solution is 0.10 mg/mL.
3. the method for micro cyanide in the dual wavelength stack spectrophotometry water according to claim 1, it is characterized in that: the buffer solution in the step (1) is potassium dihydrogen phosphate or the sodium hydroxide buffer solution of concentration 0.05 mol/L, pH value 5.8.
4. the method for micro cyanide in the dual wavelength stack spectrophotometry water according to claim 1, it is characterized in that: the preparation process of the isonicotinic acid in the step (1)-thiobarbituricacid solution is to take by weighing NaOH solution 28～30 mL that 2.0 g thiobarbituricacids and 2.5 g isonicotinic acid add 1.0 mol/L, stirs to make its dissolving back be settled to 100 mL with pure water.
5. the method for micro cyanide in the dual wavelength stack spectrophotometry water according to claim 1, it is characterized in that: step (1) toluene-sodium-sulfonchloramide solution concentration is 10.0 g/L.
CN201110174453A 2011-06-27 2011-06-27 Method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry Pending CN102262063A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
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CN103145622A (en) * 2013-03-14 2013-06-12 西北师范大学 Receptor compound for detecting cyanide ions and synthesis and application of receptor compound
CN103575685A (en) * 2013-11-11 2014-02-12 中国科学院青海盐湖研究所 Method for measuring bromide ions and iodide ions simultaneously
CN103954619A (en) * 2014-05-21 2014-07-30 江南大学 Method for quickly quantifying cyanide in white spirit
CN104165890A (en) * 2014-09-04 2014-11-26 北京智云达科技有限公司 Kit and method for rapidly detecting thiocyanate in milk and milk product
CN105823738A (en) * 2015-01-05 2016-08-03 广东省东莞市质量监督检测中心 Method for measuring content of transportable fluorescent brightener in paper product
CN106769913A (en) * 2016-11-21 2017-05-31 中国食品发酵工业研究院 The assay method of glucosides nitrile content in a kind of grain raw material
CN108195776A (en) * 2017-12-06 2018-06-22 长春黄金研究院 The assay method of cyanide in a kind of cyaniding tailing slurry
CN107144455B (en) * 2017-06-05 2019-08-06 同济大学 A kind of sample pretreating method measuring cyanide in water sample or food
CN111044507A (en) * 2019-12-10 2020-04-21 浙江新一检测科技有限公司 Method for measuring cyanide and hydrogen cyanide in workplace

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CN101256138A (en) * 2008-01-30 2008-09-03 谱尼测试科技（北京）有限公司 Method for determining soil total cyanide--isonicotinic acid--barbituric acid spectrophotometric method

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CN101256138A (en) * 2008-01-30 2008-09-03 谱尼测试科技（北京）有限公司 Method for determining soil total cyanide--isonicotinic acid--barbituric acid spectrophotometric method

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103145622A (en) * 2013-03-14 2013-06-12 西北师范大学 Receptor compound for detecting cyanide ions and synthesis and application of receptor compound
CN103145622B (en) * 2013-03-14 2014-08-13 西北师范大学 Receptor compound for detecting cyanide ions and synthesis and application of receptor compound
CN103575685A (en) * 2013-11-11 2014-02-12 中国科学院青海盐湖研究所 Method for measuring bromide ions and iodide ions simultaneously
CN103575685B (en) * 2013-11-11 2016-01-20 中国科学院青海盐湖研究所 A kind of method of Simultaneously test bromide ion and iodide ion
CN103954619A (en) * 2014-05-21 2014-07-30 江南大学 Method for quickly quantifying cyanide in white spirit
CN104165890A (en) * 2014-09-04 2014-11-26 北京智云达科技有限公司 Kit and method for rapidly detecting thiocyanate in milk and milk product
CN105823738A (en) * 2015-01-05 2016-08-03 广东省东莞市质量监督检测中心 Method for measuring content of transportable fluorescent brightener in paper product
CN105823738B (en) * 2015-01-05 2019-02-01 广东省东莞市质量监督检测中心 A kind of method of transportable property fluorescent brightener levels in measurement paper products
CN106769913A (en) * 2016-11-21 2017-05-31 中国食品发酵工业研究院 The assay method of glucosides nitrile content in a kind of grain raw material
CN107144455B (en) * 2017-06-05 2019-08-06 同济大学 A kind of sample pretreating method measuring cyanide in water sample or food
CN108195776A (en) * 2017-12-06 2018-06-22 长春黄金研究院 The assay method of cyanide in a kind of cyaniding tailing slurry
CN111044507A (en) * 2019-12-10 2020-04-21 浙江新一检测科技有限公司 Method for measuring cyanide and hydrogen cyanide in workplace

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