CN102564982A - Method for determining and correcting cyanide - Google Patents
Method for determining and correcting cyanide Download PDFInfo
- Publication number
- CN102564982A CN102564982A CN201210031390XA CN201210031390A CN102564982A CN 102564982 A CN102564982 A CN 102564982A CN 201210031390X A CN201210031390X A CN 201210031390XA CN 201210031390 A CN201210031390 A CN 201210031390A CN 102564982 A CN102564982 A CN 102564982A
- Authority
- CN
- China
- Prior art keywords
- solution
- milliliters
- mixing
- pyrazolone
- minutes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for determining and correcting cyanide. The method is characterized by comprising the following steps of: 1) putting 10 milliliters of distillate in a colorimetric tube which has a volume of 25 milliliters and is provided with a plug; 2) adding 5 milliliters of phosphate buffer solution into the tube, mixing uniformly, quickly adding 0.2 milliliter of chloramine solution, immediately inserting the plug, mixing uniformly and placing for 3 to 5 minutes; 3) adding 5 milliliters of isonicotinic acid-pyrazolone mixed solution into the tube, uniformly mixing, adding water to dilute until mixture reaches a marked line, shaking uniformly, and placing in an aqueous solution at the temperature of between 25 and 35 DEG C for 40 minutes; and 4) determining absorbance by using a cuvette with height of 1cm, and using reagent blank as reference at the wave length of 638nm, and finding out the corresponding cyanide content from the standard curve. By using an intermediate medium, the cost of purchasing, storing and managing toxic and dangerous chemicals is reduced, and potential unsafe factors of the toxic and dangerous chemicals in using operation can be reduced.
Description
Technical field:
The present invention is mainly used in the determination and analysis of prussiate in the phenol-cyanogen sewage.
Background technology:
The determination and analysis of prussiate in the phenol-cyanogen sewage generally uses the potassium cyanide standard substance to come preparing standard solution to carry out accuracy and proofreaies and correct, and promptly uses analytically pure potassium cyanide (these article are hypertoxic hazardous chemicals), is mixed with the titer of concentration known; With the detection method of using this solution is analyzed, the concentration known value of analysis result and preparation compares, and can draw the error of mensuration process again.
Because potassium cyanide is extremely toxic substance, belongs to hazardous chemical, in preserving management and operating process, all has potential insecurity.
Summary of the invention:
In order to reduce hypertoxic hazardous chemical use cost; Reduce and use danger, the present invention to propose nontoxic a kind of prussiate mensuration bearing calibration.
Technical scheme of the present invention is: introduce nontoxic intermediate medium; After the cyanide content of middle medium demarcated; The intermediate medium cyanide content of standard test; As the li material of proofreading and correct the routine analysis cyanide content, realization is quoted the standard substance standard value, reduces cost and the danger of directly using severe toxicity and hazardous chemical potassium cyanide.
Be to reduce the error that intermediate medium is quoted standard substance, use under the steady production condition at the water sample of surveying as intermediate material.
Described steady production condition is: when gathering water sample, produce no abnormal fluctuation, promptly water sample can be represented the horizontal index of ordinary production.
Prussiate is measured program (low concentration in the waste water):
The instrument that the present invention adopted has:
1500 milliliters of full glass distillers; Distillate conduit (the distillate conduit inserts in the absorption liquid of receiving bottle); Receiving bottle; Spectrophotometer; 25 milliliters of color-comparison tubes.
The reagent that the present invention adopted has:
15% tartaric acid solution: promptly get 15 gram tartrate and be dissolved in 100 ml waters;
2% sodium hydroxide solution: promptly get 2 gram NaOH and be dissolved in 100 ml waters;
0.05% methyl orange indicator solution;
Zinc nitrate solution: promptly get 10 gram zinc nitrates and be dissolved in 100 ml waters;
PBS (PH=7): i.e. weighing 34 gram anhydrous potassium dihydrogenphosphates and 35.5 gram ADSPs are in beaker, and being dissolved in water is diluted in 1000 ml waters, shakes up;
Gansil solution: promptly face with before, taking by weighing 0.1 gram, gansil is water-soluble is diluted to 100 milliliters, shakes up, and contains in brown bottle;
Isonicotinic acid-pyrazolone solution;
Isonicotinic acid solution: promptly take by weighing 1.5 gram isonicotinic acid and be dissolved in 24 milliliters of sodium hydroxide solutions thin up to 100 milliliter;
Pyrazolone solution: promptly take by weighing 0.25 gram pyrazolone and be dissolved in 20 milliliters of dimethylformamides.Face with preceding pyrazolone and isonicotinic acid solution are mixed according to 1:5.
Technical scheme of the present invention is: in water sample, add tartrate and trbasic zinc phosphate; Under the condition of pH4 (being that the water potential of hydrogen is pH=4), add thermal distillation; Simple prussiate and part complexing cyanogen are distilled out, and the simple prussiate that distills out is used colorimetric method for determining content after sodium hydroxide solution absorbs; Under neutrallty condition, simple prussiate in the water sample and gansil reaction generate cyanogen chloride, again with the isonicotinic acid effect, after hydrolysis, generate the pentaene dialdehyde, and last and pyrazolone condensation generates blue dyes, and its colourity is directly proportional with the content of prussiate.
Concrete operations step of the present invention is:
1, gets 10 milliliters of distillates in 25 milliliters of color-comparison tubes;
2, Xiang Guanzhong adds 5 milliliters of PBSs, and mixing adds 0.2 milliliter of gansil solution rapidly, capping plug immediately, and mixing was placed 3-5 minutes;
3, Xiang Guanzhong adds 5 milliliters of isonicotinic acid-pyrazolone mixed solution, and mixing, thin up shake up to graticule, in 25-35 ℃ of WS, places 40 minutes;
4, at wavelength 638nm place, using the 1cm cuvette, is reference with the reagent blank, measures absorbance, finds corresponding cyanide content from typical curve.
The present invention uses reality surveying the water sample as intermediate medium, and sampling is convenient, and method of operating is simple, and easy master can reduce correction error in the trimming process; Reduced and used purchasing, taking care of and handling cost of hypertoxic chemicals; Reduced the danger of using hypertoxic dangerous material.
Embodiment:
Concrete operations step of the present invention is:
1, gets 10 milliliters of distillates in 25 milliliters of color-comparison tubes;
2, Xiang Guanzhong adds 5 milliliters of PBSs, and mixing adds 0.2 milliliter of gansil solution rapidly, capping plug immediately, and mixing was placed 3-5 minutes;
3, Xiang Guanzhong adds 5 milliliters of isonicotinic acid-pyrazolone mixed solution, and mixing, thin up shake up to graticule, in 25-35 ℃ of WS, places 40 minutes;
4, at wavelength 638nm place, using the 1cm cuvette, is reference with the reagent blank, measures absorbance, finds corresponding cyanide content from typical curve.
Points for attention in the aforesaid operations step:
When 1, gathering the water sample of measuring prussiate, must add alkali and fix, add solid NaOH to PH＞12.
2, the water sample of prussiate should be measured in the sky as early as possible.
3, prussiate volatilizees easily, and therefore, each step all will be operated rapidly after the acidifying, and covers completely at any time.
Claims (1)
1. a prussiate is measured bearing calibration, comprises following reagent: 15% tartaric acid solution; 2% sodium hydroxide solution; 0.05% methyl orange indicator solution; Zinc nitrate solution; PBS; Gansil solution; Isonicotinic acid-pyrazolone solution; Isonicotinic acid solution; Pyrazolone solution,
It is characterized in that comprising following operation steps:
(1), gets 10 milliliters of distillates in 25 milliliters of color-comparison tubes;
(2), Xiang Guanzhong adds 5 milliliters of PBSs, mixing adds 0.2 milliliter of gansil solution rapidly, capping plug immediately, mixing was placed 3-5 minutes;
(3), Xiang Guanzhong adds 5 milliliters of isonicotinic acid-pyrazolone mixed solution, mixing, thin up shake up to graticule, in 25-35 ℃ of WS, place 40 minutes;
(4), at wavelength 638nm place, use the 1cm cuvette, be reference with the reagent blank, measure absorbance, find corresponding cyanide content from typical curve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210031390XA CN102564982A (en) | 2012-02-13 | 2012-02-13 | Method for determining and correcting cyanide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210031390XA CN102564982A (en) | 2012-02-13 | 2012-02-13 | Method for determining and correcting cyanide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102564982A true CN102564982A (en) | 2012-07-11 |
Family
ID=46410973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210031390XA Pending CN102564982A (en) | 2012-02-13 | 2012-02-13 | Method for determining and correcting cyanide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102564982A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954619A (en) * | 2014-05-21 | 2014-07-30 | 江南大学 | Method for quickly quantifying cyanide in white spirit |
| 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 |
| CN107703072A (en) * | 2017-09-21 | 2018-02-16 | 长春黄金研究院 | The correction assay method of total cyanide in a kind of thiocyanate water quality |
| CN107817220A (en) * | 2017-11-29 | 2018-03-20 | 长春黄金研究院 | The assay method of easy release cyanide mass concentration in thiocyanate water quality |
| CN107991429A (en) * | 2017-11-29 | 2018-05-04 | 长春黄金研究院 | The assay method of cyanide is easily discharged in a kind of cyanide wastewater of sulfur compound |
| 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 |
-
2012
- 2012-02-13 CN CN201210031390XA patent/CN102564982A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 任占军 等: "异烟酸一吡唑啉酮光度法测定水中氰化物的方法改进", 《现代仪器》 * |
| 潘河 等: "异烟酸－吡唑啉酮分光光度法测定地下水中氰化物的不确定度评定", 《岩矿测试》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103954619A (en) * | 2014-05-21 | 2014-07-30 | 江南大学 | Method for quickly quantifying cyanide in white spirit |
| 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 |
| CN107703072A (en) * | 2017-09-21 | 2018-02-16 | 长春黄金研究院 | The correction assay method of total cyanide in a kind of thiocyanate water quality |
| CN107817220A (en) * | 2017-11-29 | 2018-03-20 | 长春黄金研究院 | The assay method of easy release cyanide mass concentration in thiocyanate water quality |
| CN107991429A (en) * | 2017-11-29 | 2018-05-04 | 长春黄金研究院 | The assay method of cyanide is easily discharged in a kind of cyanide wastewater of sulfur compound |
| CN107991429B (en) * | 2017-11-29 | 2020-04-24 | 长春黄金研究院 | Method for determining cyanide easily released in cyanide-containing wastewater containing sulfide |
| CN107817220B (en) * | 2017-11-29 | 2020-11-24 | 长春黄金研究院有限公司 | Method for measuring mass concentration of easily released cyanide in thiocyanate-containing water |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102564982A (en) | Method for determining and correcting cyanide | |
| CN106841056A (en) | A kind of detection method of formaldehyde content in indoor air | |
| CA2806491A1 (en) | Simultaneous determination of multiple analytes in industrial water system | |
| CN110987918A (en) | Detection reagent and rapid detection method for total nitrogen in water | |
| CN109612951A (en) | For detecting chlorine residue in water/total chlorine detection agent and preparation method thereof and detection method | |
| CN103439279B (en) | Spectrophotometry quantitative analysis method of iodine-starch color-developing system | |
| CN100422718C (en) | Method for determining sodium chloride content in phosphate using spectrophotometry | |
| KR20070073682A (en) | Kit for measuring hardness of water and detection method using the same | |
| CN107817220B (en) | Method for measuring mass concentration of easily released cyanide in thiocyanate-containing water | |
| CN104142323A (en) | Method for simultaneously measuring content of nitrogen and phosphorus of plant | |
| CN101900671B (en) | Method for fast measuring ozone in water and apparatus thereof | |
| CN102323226A (en) | A kind of method of measuring three nitrogen concentrations in the water | |
| CN104062396A (en) | Method for measuring content of nitrogen in metal lithium and lithium alloy | |
| JP4273184B2 (en) | Phosphate measurement method and apparatus | |
| CN103472015A (en) | Dynamic absorbance quantitative analysis method based on iodine-starch chromogenic system | |
| Hydes et al. | Report on a desk study to identify likely sources of error in the measurements of carbonate system parameters and related calculations, particularly with respect to coastal waters and ocean acidification experiments. Supplement to DEFRA contract ME4133 “DEFRApH monitoring project” | |
| CN107884402A (en) | The method of the fast test tube of hydrogen peroxide integration and quick detection hydrogen peroxide | |
| Jackson et al. | Sodium Chlorite as a Volumetric Oxidizing Agent | |
| US10620129B1 (en) | Systems and methods for determining carbon system parameters of water | |
| CN103376302B (en) | A kind of measurement method of carbonaceous organic material | |
| Yuan et al. | A simple and cost‐effective manual solid phase extraction method for the determination of nanomolar dissolved reactive phosphorus in aqueous samples | |
| CN103018184B (en) | A kind of method measuring underwater trace bromate | |
| Tkáčová et al. | Determination of chlorine dioxide and chlorite in water supply systems by verified methods | |
| CN105181410A (en) | Method for determining formaldehyde content in N-hydroxymethyl methionine calcium product | |
| Fontela et al. | Carbonate system species and pH |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120711 |