CN101256138A - Method for determining soil total cyanide--isonicotinic acid--barbituric acid spectrophotometric method - Google Patents
Method for determining soil total cyanide--isonicotinic acid--barbituric acid spectrophotometric method Download PDFInfo
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- CN101256138A CN101256138A CNA2008100571411A CN200810057141A CN101256138A CN 101256138 A CN101256138 A CN 101256138A CN A2008100571411 A CNA2008100571411 A CN A2008100571411A CN 200810057141 A CN200810057141 A CN 200810057141A CN 101256138 A CN101256138 A CN 101256138A
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- barbiturates
- total cyanide
- isonicotinic acid
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- spectrophotometric
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Abstract
The invention provides a test method, which includes the following steps: distilling soil in pH<2 acidic medium, hydrogen cyanide is formed, absorbing with the sodium hydrate solution, and analyzing total cyanide in soil with isonicotinic acid-barbituric acid spectrophotometry. The invention has the advantages of good sensitivity and good repeatability, which provides a convenient and reliable method for analyzing total cyanide in soil, and meets the needs of soil pollutant analysis as well as research work.
Description
Technical field
The present invention relates to the assay method of soil total cyanide, is a kind of a kind of assay method that develops the color, uses the ultraviolet-visible spectrophotometer quantitative test with isonicotinic acid-barbiturates.
Background technology
Prussiate belongs to extremely toxic substance, mainly is to combine with ferricytochrome oxidase to the toxicity of human body, generates cyanocytochromeoxidase and loses the effect of transmitting oxygen, causes that histanoxia suffocates.The main source of prussiate is artificial pollution source in the soil, reach the soil resource in downstream near the industrial wastewater pollutions such as the exploitation of for example little gold mine, smelting, plating, organic chemical industry, ore dressing, people can constitute harm greatly to people's health when using these land resources.Country's isonicotinic acid also of no use-barbiturates spectrophotometric method is analyzed the method for soil total cyanide at present, and therefore, the invention of this method is for people analyze, the research soil total cyanide provides a convenience, reliable method.
Summary of the invention
Technical matters to be solved by this invention is, in the presence of phosphoric acid and EDTA, in the acid medium of PH＜2, adds the prussiate that thermal distillation can generate hydrogen cyanide, comprises all simple prussiate and most complex cyanide.
For achieving the above object, the present invention takes following design proposal:
The assay method of soil total cyanide of the present invention--isonicotinic acid-barbiturates spectrophotometric method is characterized in that this method comprises the steps:
(1) takes by weighing the distilling flask that 5～10g pedotheque to be measured (specifically fixed by cyanide content) places 500mL, add the distilled water of 200mL, several beaded glasses.
(2) in distilling flask, add 10mLNa
2-EDTA solution and 7～8 methyl orange indicators.
(3) add in the receiving bottle (100mL graduated cylinder) 10mL concentration be 1% sodium hydroxide solution as absorption liquid, termination condenser pipe outlet on the distillate conduit, 1cm is at least inserted under the absorption liquid of receiving flask in the lower end.
(4) in distilling flask, add 10mL phosphoric acid rapidly, make PH＜2, build bottle stopper immediately.
(5) open condensate water, regulate adjustable electric furnace, add thermal distillation, and the solution of maintenance cucurbit is red in still-process with 2～4mL/min distillate speed.
(6) stop distillation during near 100ml when solution in the receiving bottle,, take out receiving bottle, be settled to graticule with a small amount of distilled water with a small amount of distillation washing distillate conduit.This alkaline distillate is used for measuring total cyanide.
(7) assay method of soil total cyanide--isonicotinic acid-barbiturates spectrophotometric method, the method for drafting of calibration curve is as follows:
1. get 8 25mL color-comparison tubes, add the potassium cyanide standard respectively and use liquid (1mL contains CN-1.00 μ g) 0.00,0.20,0.50,1.00,2.00,3.00,4.00,5.00mL, each adds concentration is that 0.1% NaOH solution is to 10mL.
2. each pipe adds 5mLKH
2PO
4(PH=4.0) solution, mixing, adding 0.30mL concentration rapidly is 1% toluene-sodium-sulfonchloramide, capping plug immediately, slowly mixing was placed 1～2 minute.
3. respectively pipe adds 6.0mL isonicotinic acid-barbiturates developer, is diluted with water to groove, and the capping plug mixing is in 25 ℃ of colour developings 15 minutes (15 ℃ were developed the color 25 minutes, and 30 ℃ were developed the color 10 minutes).
4. on ultraviolet-visible spectrophotometer, in 600nm wavelength place, make reference, measure and respectively manage absorbance, with CN with zero-dose blank solution pipe with the 1cm cuvette
-Content (μ g) is horizontal ordinate, is ordinate with the absorbance, the drawing standard curve.
(8) draw 10.00mL sample distillate and 10.00mL blank test distillate respectively in the 25mL color-comparison tube, carry out the absorbance of working sample by plot step (2)～(4) of typical curve.
(9) computing method of soil total cyanide are as follows:
In the formula: m
1---soil sample total cyanide content (μ g)
The m---pre-distillation is handled the quality (g) of used pedotheque
V
1--the volume (mL) of-sample distillate
V
2---be used to the develop the color volume (mL) of institute's sample thief distillate
Advantage of the present invention is: adopt isonicotinic acid-barbiturates spectrophotometric method to detect total cyanide concentration in the soil, easily and fast, relative standard deviation detects and is limited to 0.5mg/kg less than 5%.This shows that this method is for detecting total cyanide concentration in the soil, a kind of method of implementing be convenient to reliably is provided, can satisfy soil pollutant analysis and research work needs.
Embodiment
Embodiment 1, the detection of pedotheque 1# total cyanide concentration:
Take by weighing pedotheque 1# 5.1079g to be measured, in the distilling flask of 500mL, add the distilled water of 200mL, several beaded glasses.Add 10mLNa at distilling flask
2-EDTA solution and 7～8 methyl orange indicators.Add 10mL concentration in the receiving bottle (100mL graduated cylinder) and be 1% sodium hydroxide solution as absorption liquid, termination condenser pipe outlet on the distillate conduit, 1cm is at least inserted below the absorption liquid of receiving flask in the lower end.In distilling flask, add 10mL phosphoric acid rapidly, make PH＜2, build bottle stopper immediately.Open condensate water, regulate adjustable electric furnace, add thermal distillation, and keep the solution of cucurbit to keep red with 2～4mL/min distillate speed.When solution in the receiving bottle stops distillation during near 100ml, with a small amount of distillation washing distillate conduit, take out receiving bottle, be settled to graticule with a small amount of distilled water.This alkaline distillate is used for measuring total cyanide.
Assay method according to soil total cyanide--isonicotinic acid-barbiturates spectrophotometric method, draw following typical curve:
| CN -(μg) | 0.00 | 0.20 | 0.50 | 1.00 | 2.00 | 3.00 | 4.00 | 5.00 |
| Absorbance (A) | 0.000 | 0.012 | 0.047 | 0.092 | 0.212 | 0.330 | 0.450 | 0.579 |
Curve's equation: Y=0.117x-0.0158
Related coefficient: R=0.9991
Draw 6 parts of 10.00mL sample distillates and 10.00mL blank test distillate, place the 25mL color-comparison tube respectively, undertaken by plot step (2)～(4) of typical curve, the absorbance of working sample calculates the concentration of pedotheque total cyanide.
| Soil sample 1# | 1#-1 | 1#-2 | 1#-3 | 1#-4 | 1#-5 | 1#-6 | RSD/％ |
| CN -(mg/Kg) | 2.34 | 2.25 | 2.47 | 2.24 | 2.36 | 2.44 | 3.7 |
The detection of embodiment 2 pedotheque 2# total cyanide concentration:
Take by weighing pedotheque 2# 10.0014g to be measured, in the distilling flask of 500mL, add the distilled water of 200mL, several beaded glasses.Add 10mLNa at distilling flask
2-EDTA solution and 7～8 methyl orange indicators.Add 10mL concentration in the receiving bottle (100mL graduated cylinder) and be 1% sodium hydroxide solution as absorption liquid, termination condenser pipe outlet on the distillate conduit, 1cm is at least inserted below the absorption liquid of receiving flask in the lower end.In distilling flask, add 10mL phosphoric acid rapidly, make PH＜2, build bottle stopper immediately.Open condensate water, regulate adjustable electric furnace, add thermal distillation, and keep the solution of cucurbit to keep red with 2～4mL/min distillate speed.When solution in the receiving bottle stops distillation during near 100ml, with a small amount of distillation washing distillate conduit, take out receiving bottle, be settled to graticule with a small amount of distilled water.This alkaline distillate is used for measuring total cyanide.
Assay method according to soil total cyanide--isonicotinic acid-barbiturates spectrophotometric method, draw following typical curve:
| CN -(μg) | 0.00 | 0.20 | 0.50 | 1.00 | 2.00 | 3.00 | 4.00 | 5.00 |
| Absorbance (A) | 0.000 | 0.014 | 0.048 | 0.087 | 0.213 | 0.332 | 0.451 | 0.576 |
Curve's equation: Y=0.1168x-0.0155
Related coefficient: R=0.9990
Draw 6 parts of 10.00mL sample distillates and 10.00mL blank test distillate, place the 25mL color-comparison tube respectively, undertaken by plot step (2)～(4) of typical curve, the absorbance of working sample calculates the concentration of pedotheque total cyanide.
| Soil sample 2# | 2#-1 | 2#-2 | 2#-3 | 2#-4 | 2#-5 | 2#-6 | RSD/％ |
| CN -(mg/Kg) | 1.07 | 1.14 | 1.09 | 1.15 | 1.02 | 1.13 | 4.1 |
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (9)
1, the assay method of soil total cyanide--isonicotinic acid-barbiturates spectrophotometric method is characterized in that this method comprises the steps:
Take by weighing an amount of pedotheque to be measured (it is fixed specifically to press cyanide content) in the distilling flask of 500mL, add the distilled water of 100～200mL and an amount of Na
2-EDTA solution distills in acid medium, forms hydrogen cyanide, with the sodium hydroxide solution absorption of an amount of concentration, adopts the total cyanide in isonicotinic acid-barbiturates spectrophotometric analysis soil.
Result of calculation, the computing formula of total cyanide is in the sample:
In the formula: m
1---soil sample total cyanide content (μ g)
The m---pre-distillation is handled the quality (g) of used pedotheque
V
1--the volume (mL) of-sample distillate
V
2---be used to the develop the color volume (mL) of institute's sample thief distillate
2, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: utilize isonicotinic acid-barbiturates spectrophotometric method to carry out the mensuration of soil total cyanide;
3, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: the amount of taking by weighing of pedotheque to be measured is 5～10g, and concrete sample weighting amount is decided according to cyanide content;
4, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: add 200mL distilled water in the distilling flask;
5, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: adding 10mL concentration is 10% Na
2-EDTA solution and 7～8 methyl orange indicators;
6, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: add 10ml phosphoric acid rapidly in distilling flask, make PH＜2 of acid medium;
7, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: absorbent solution is that concentration is 1% sodium hydroxide solution;
8, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: distillation speed is 2～4mL/min distillate;
9, the assay method of soil total cyanide according to claim 1--isonicotinic acid-barbiturates spectrophotometric method is characterized in that: keep the solution in the cucurbit to be redness in still-process.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033065A (en) * | 2010-11-27 | 2011-04-27 | 大连大学 | Digital colorimetric method for measuring cyanide concentration in environment and biological sample |
| CN102262063A (en) * | 2011-06-27 | 2011-11-30 | 吴佑琼 | Method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry |
| CN102621137A (en) * | 2012-03-14 | 2012-08-01 | 华东理工大学 | Detection reagent for fast detecting cyanide in water and preparation method of detection reagent |
| CN103901032A (en) * | 2014-04-16 | 2014-07-02 | 北京瑞升特科技有限公司 | Method and system for vaccine detection |
| 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 |
| CN104931498A (en) * | 2015-06-30 | 2015-09-23 | 苏州东辰林达检测技术有限公司 | Hydrogen cyanide detection reagent and preparation method thereof |
| CN106370647A (en) * | 2016-08-18 | 2017-02-01 | 安徽瑞思威尔科技有限公司 | Highly flavored type liquor base cyanide analysis pre-treatment method |
| CN107167472A (en) * | 2017-05-08 | 2017-09-15 | 长春黄金研究院 | The rapid assay methods of total cyanide in a kind of ore pulp containing cyanogen |
| 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 |
| CN108254488A (en) * | 2018-01-21 | 2018-07-06 | 长春黄金研究院有限公司 | Thiocyanate, sulfide solid waste in total cyanide assay method |
| CN108303492A (en) * | 2018-01-21 | 2018-07-20 | 长春黄金研究院有限公司 | The assay method of cyanide is easily discharged in a kind of solid waste containing cyanogen of sulfur compound |
| 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 |
| CN111879765A (en) * | 2020-07-21 | 2020-11-03 | 韩文红 | Method for measuring volatile phenol and cyanide in water quality, soil or municipal sludge |
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2008
- 2008-01-30 CN CNA2008100571411A patent/CN101256138A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102033065A (en) * | 2010-11-27 | 2011-04-27 | 大连大学 | Digital colorimetric method for measuring cyanide concentration in environment and biological sample |
| CN102262063A (en) * | 2011-06-27 | 2011-11-30 | 吴佑琼 | Method for measuring trace quantity of prussiate in water by using dual-wavelength superposition spectrophotometry |
| CN102621137A (en) * | 2012-03-14 | 2012-08-01 | 华东理工大学 | Detection reagent for fast detecting cyanide in water and preparation method of detection reagent |
| CN102621137B (en) * | 2012-03-14 | 2014-10-29 | 华东理工大学 | Detection reagent for fast detecting cyanide in water and preparation method of detection reagent |
| CN103901032A (en) * | 2014-04-16 | 2014-07-02 | 北京瑞升特科技有限公司 | Method and system for vaccine detection |
| 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 |
| CN104931498A (en) * | 2015-06-30 | 2015-09-23 | 苏州东辰林达检测技术有限公司 | Hydrogen cyanide detection reagent and preparation method thereof |
| CN106370647A (en) * | 2016-08-18 | 2017-02-01 | 安徽瑞思威尔科技有限公司 | Highly flavored type liquor base cyanide analysis pre-treatment method |
| CN107167472A (en) * | 2017-05-08 | 2017-09-15 | 长春黄金研究院 | The rapid assay methods of total cyanide in a kind of ore pulp containing cyanogen |
| CN107167472B (en) * | 2017-05-08 | 2019-12-03 | 长春黄金研究院 | The rapid assay methods of total cyanide in a kind of ore pulp containing cyanogen |
| 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 |
| CN108254488A (en) * | 2018-01-21 | 2018-07-06 | 长春黄金研究院有限公司 | Thiocyanate, sulfide solid waste in total cyanide assay method |
| CN108303492A (en) * | 2018-01-21 | 2018-07-20 | 长春黄金研究院有限公司 | The assay method of cyanide is easily discharged in a kind of solid waste containing cyanogen of sulfur compound |
| CN111879765A (en) * | 2020-07-21 | 2020-11-03 | 韩文红 | Method for measuring volatile phenol and cyanide in water quality, soil or municipal sludge |
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