CN115728443B - Method for measuring cyanide ions in complex water quality - Google Patents
Method for measuring cyanide ions in complex water quality Download PDFInfo
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- CN115728443B CN115728443B CN202310036284.9A CN202310036284A CN115728443B CN 115728443 B CN115728443 B CN 115728443B CN 202310036284 A CN202310036284 A CN 202310036284A CN 115728443 B CN115728443 B CN 115728443B
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Abstract
The invention provides a method for determining cyanide ions in complex water quality, which comprises the steps of firstly adding ascorbic acid into a diluent of a water sample to be tested under the water bath condition of 50-70 ℃, eliminating possible oxidizing substances in the water quality, then introducing nitrogen to blow off the cyanide ions in the form of HCN, passing the blown-off HCN through lead acetate cotton, absorbing the blown-off HCN by using sodium hydroxide absorption liquid, and then titrating by using silver nitrate solution by taking rhodanine as an indicator, thus accurately determining the content of the cyanide ions in the water sample to be tested. In the process, the free cyanide ions are removed from the water sample in the form of HCN, and then analysis and determination are carried out, so that the influence of interfering ions or substances in the water sample on the cyanide ions is effectively eliminated, and the accuracy of determining the cyanide ions is improved. Analysis and measurement results show that the measurement results of the method provided by the invention have the advantages of good parallelism and high accuracy.
Description
Technical Field
The invention relates to the technical field of a method for measuring cyanide ions in a cyanide process in the gold industry, in particular to a method for measuring cyanide ions in complex water quality.
Background
The cyanide gold extraction process is that cyanide is used as leaching solution to extract gold, and is the main method for extracting gold from ore or concentrate. In the above process, sodium cyanide is added into the system to be extracted to make gold use of cyanide ion to make Au (CN) 2- The complex ion form is selected, thereby achieving the purpose of gold extraction. The water is generally added as mine cyanide backwater, which itself contains a certain cyanide, and the cyanide includes cyanide in the form of iron cyanide complex, copper cyanide complex, zinc cyanide complex and the like in the form of complexation, and also includes cyanide in the form of cyanide ions. However, the cyanide existing in the cyanide ion form is only often used for extracting gold in the cyanide gold extraction process, and the accurate content of cyanide ions in water can be determined by measuring the cyanide existing in the cyanide ion form, and the amount of sodium cyanide required to be added in the gold extraction process can be determined by calculation. The method has important guiding effect on the addition amount of sodium cyanide in the gold extraction process, and has important significance on environmental protection and carbon emission. In addition, the cyanide ion determination process is easily affected by other interference ions, so that the determination result is inaccurate, and the composition of a water sample is more complex in complex water quality such as gold extraction process wastewater, and the difficulty of accurately determining the cyanide ions in the water sample is increased.
In view of the above, there is a need to design an improved method for measuring cyanide ions in complex water quality to solve the above problems.
Disclosure of Invention
The invention aims to provide a method for measuring cyanide ions in complex water quality.
In order to achieve the aim of the invention, the invention provides a method for measuring cyanide ions in complex water quality, which comprises the following steps:
s1, taking a proper amount of water sample into a reaction bottle, adding water to dilute the water sample to 200mL, adding ascorbic acid and phenolphthalein solution under the water bath condition, and adjusting the solution to be alkaline by using a first sodium hydroxide solution; then, connecting a pipeline, enabling the outlet end of the air duct to be inserted into sodium hydroxide absorption liquid, adding concentrated phosphoric acid into the reaction bottle, rapidly introducing nitrogen into the reaction bottle, and adjusting the flow of the nitrogen to enable cyanide ions to be blown off in a HCN mode;
s2, transferring the sodium hydroxide absorption liquid with HCN absorbed in the step S1 into a distillation flask, adding a second sodium hydroxide solution, stannous chloride solution, copper sulfate solution and the concentrated phosphoric acid, absorbing the distillate by using a third sodium hydroxide solution with the concentration of 2%, distilling to 100mL, and stopping heating;
s3, after the distillate obtained in the step S2 is subjected to distillation treatment to a constant volume, titrating with a silver nitrate solution by taking rhodanine as an indicator, and calculating the cyanide ion content.
Preferably, in step S1, lead acetate cotton is placed in the air duct at the front end of the sodium hydroxide absorption liquid.
Preferably, in step S1, the temperature range of the water bath condition is 50-70 ℃.
Preferably, in the step S2, the mass concentration of the second sodium hydroxide solution is 100g/L, and the adding amount is 3.0mL; the concentration of the stannous chloride solution is 50g/L, and the adding amount is 2.0mL; the concentration of the copper sulfate solution is 200g/L, and the addition amount is 10mL; the addition amount of the concentrated phosphoric acid is 10mL.
Preferably, in the step S2, the speed of blowing nitrogen is 350-500 mL/min, the purity of the nitrogen is 99.99%, and the blowing time is 30min.
Preferably, in step S1, the concentration of the ascorbic acid is 1%, and the addition amount is 5.0mL.
Preferably, in step S1, the preparation method of the lead acetate cotton is as follows: 10g of lead acetate is dissolved in 100mL of water to obtain a lead acetate solution, and 10g of absorbent cotton is soaked in the lead acetate solution and taken out for airing.
Preferably, in step S1, the concentration of the sodium hydroxide absorption solution is 5.0g/L.
Preferably, in step S1, the amount of the concentrated phosphoric acid added is 10mL.
Preferably, in step S3, the concentration of the silver nitrate solution is 0.0100mol/L.
The beneficial effects of the invention are as follows:
1. according to the method for determining the cyanide ions in the complex water quality, provided by the invention, the ascorbic acid is firstly added into the diluent of the water sample to be tested under the water bath condition of 50-70 ℃, so that possible oxidizing substances in the water quality are eliminated, then nitrogen is introduced to blow off the cyanide ions in the form of HCN, the blown-off HCN passes through lead acetate cotton, then sodium hydroxide absorption liquid is used for absorbing the blown-off HCN, and then the rhodanine is used as an indicator, and the silver nitrate solution is used for titration, so that the cyanide ion content in the water sample to be tested can be accurately determined. In the process, the free cyanide ions are removed from the water sample in the form of HCN, and then analysis and determination are carried out, so that the influence of interfering ions or substances in the water sample on the cyanide ions is effectively eliminated, and the accuracy of determining the cyanide ions is improved.
2. According to the method for determining cyanide ions in complex water quality, provided by the invention, the interference of sulfides on cyanide ions during acidification and stripping is eliminated by adding lead acetate, and the interference of other interference ions or substances such as sulfides is further eliminated by adding stannous chloride and copper sulfate; the cyanide ions are further purified by adding concentrated phosphoric acid and then carrying out distillation operation, so that the interference of the subsequent titration process is eliminated, and the accuracy of measurement is ensured. Analysis and measurement results show that the measurement results of the method provided by the invention have the advantages of good parallelism and high accuracy. In addition, the method can accurately measure the cyanide ion concentration in complex water such as cyanide backwater, barren liquor and the like, provides an effective metering mode for the addition of sodium cyanide in the gold extraction process in the gold industry, and has important significance on environmental protection and carbon emission.
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FIG. 1 is a flow chart of a method for measuring cyanide ions in complex water quality.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
It should be noted that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to aspects of the present invention are shown in the drawings, and other details not greatly related to the present invention are omitted.
In addition, it should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Referring to fig. 1, the method for determining cyanide ions in complex water provided by the invention comprises the following steps:
s1, taking a proper amount of water sample into a reaction bottle, adding water to dilute the water sample to 200mL, adding ascorbic acid and phenolphthalein solution under the water bath condition, and adjusting the solution to be alkaline by using sodium hydroxide solution; then, putting the initial end of the air duct into lead acetate cotton, inserting the outlet end of the air duct into sodium hydroxide absorption liquid, adding 10mL of concentrated phosphoric acid into a reaction bottle, rapidly introducing nitrogen into the reaction bottle, adjusting the flow of the nitrogen, and continuously blowing nitrogen into the reaction bottle at a speed of 350-500 mL/min for 30min to ensure that cyanide ions are blown off in a HCN form;
s2, transferring the sodium hydroxide absorption liquid with the HCN absorbed in the step S1 into a distillation flask, adding sodium hydroxide solution, stannous chloride solution, copper sulfate solution and concentrated phosphoric acid, absorbing the distillate with 2% sodium hydroxide solution, distilling to 100mL, and stopping heating;
s3, after the distillate obtained in the step S2 is subjected to distillation treatment to a constant volume, titrating with a silver nitrate solution by taking rhodanine as an indicator, and calculating the cyanide ion content.
Preferably, in the step S1, the temperature range of the water bath condition is 50-70 ℃, and under the temperature range, the release of cyanide in a complexation form can be effectively avoided, and the accuracy of the subsequent measurement result is influenced.
Preferably, in step S1, the concentration of ascorbic acid is 1% and the addition amount is 5.0mL; according to the acidity of the sample, sodium hydroxide solution with mass concentration of 2% or 40% is selected to adjust the pH value of the solution until the solution just shows red, and 10mL of 2% sodium hydroxide solution is added.
Preferably, in step S1, the lead acetate cotton is prepared by the following steps: 10g of lead acetate was dissolved in 100mL of water to obtain a lead acetate solution, and 10g of absorbent cotton was immersed in the lead acetate solution to be soaked, taken out and dried.
Preferably, in step S1, the concentration of the sodium hydroxide absorbing solution is 5.0g/L, and the specific volume is set according to the amount of cyanide ions in the water sample at the time of actual measurement, so long as effective absorption of cyanide ions can be ensured, which is not limited thereto.
Preferably, in step S1, the amount of concentrated phosphoric acid added is 10mL; the purity of the nitrogen is 99.99%, and the blowing time is 30min.
Preferably, in step S2, the mass concentration of the sodium hydroxide solution is 100g/L, and the addition amount is 3.0mL; stannous chloride concentration is 50g/L, and the addition amount is 2.0mL; the concentration of the copper sulfate is 200g/L, and the addition amount is 10mL; the addition amount of concentrated phosphoric acid was 10mL.
Preferably, in step S3, the concentration of the silver nitrate solution is 0.010 mol/L, and the specific addition amount thereof depends on the content of cyanide ions during titration.
The method for measuring cyanide ions in complex water quality according to the invention is further described below with reference to specific examples:
example 1
In this embodiment, a gold mine barren solution is used as a measuring object, and the method of the present invention is used for measuring the concentration of cyanide ions in the water quality, and the specific measuring process includes the following steps:
s1, taking 50mL of water sample, diluting to 200mL, adding 5.0mL of 1% ascorbic acid under the water bath condition of 60 ℃, adding phenolphthalein solution, and adjusting the solution to red by sodium hydroxide; then, connecting a pipeline, putting the initial end of an air duct into lead acetate cotton, inserting the outlet end of the air duct into 40mL of sodium hydroxide absorption liquid with the concentration of 5.0g/L, adding 10mL of concentrated phosphoric acid into a reaction bottle, rapidly introducing nitrogen into the reaction bottle, adjusting the flow of the nitrogen, and continuously blowing nitrogen into the reaction bottle at the speed of 350-500 mL/min for 30min to ensure that cyanide ions are blown off in the form of HCN;
s2, transferring the sodium hydroxide absorption liquid absorbed with HCN in the step S1 into a distillation flask, adding 3.0mL of 100g/L sodium hydroxide solution, 2.0mL of 50g/L stannous chloride solution, 10mL of 200g/L copper sulfate solution and 10mL of concentrated phosphoric acid, absorbing the distillate with 2% sodium hydroxide solution, distilling to 100mL, and stopping heating;
s3, after the distillate obtained in the step S2 is subjected to distillation treatment to a constant volume, transferring all the distillate into a 250mL conical flask, titrating with a silver nitrate solution by taking rhodanine as an indicator, and calculating the cyanide ion content; in the measurement process, deionized water is used as a blank test, and the cyanide ion concentration is calculated to be 54.4mg/L.
Example 2
In this example, cyanide ions in the recovery of a gold mine process are used as the measurement object, and the difference in example 1 is that: in the step S1, 100mL of water sample is taken as an experimental determination object, a solution diluted to 200mL by adding water is taken as an experimental determination object, other steps are basically the same as those of the embodiment 1, and are not repeated herein, deionized water is taken as a blank test in the determination process, and the cyanide ion concentration measured in the embodiment is 23.6mg/L.
Example 3
In order to verify the accuracy of the method for measuring cyanide ions in complex water quality, the invention adopts a mixed solution prepared from sodium cyanide, potassium ferricyanide, potassium thiocyanate and sodium sulfide as a measurement water sample; wherein the concentration of cyanide ions in the mixed solution is 20.0mg/L, the concentration of ferricyanide compounds (calculated as cyanide) is 50.0mg/L, the concentration of potassium thiocyanate is 200mg/L, and the concentration of sulfide is 200mg/L. The method for measuring the cyanide ion concentration in the water sample in the embodiment 1 is basically the same as the method for measuring the cyanide ion concentration in the water sample in the embodiment 1, and the specific measurement steps are not repeated herein, deionized water is used as a blank test in the measurement process, four groups of the deionized water are measured in parallel, the measured cyanide ion concentrations are respectively 14.4mg/L, 14.7mg/L, 14.8mg/L and 14.6mg/L, the cyanide ion recovery rate is 96.0-98.7%, and the result shows that when the method for measuring the cyanide ion in the water sample with complex composition is used, the influence of other interference ions such as sulfur ions can be effectively eliminated, and the measurement result has the advantages of good parallelism and high accuracy.
Example 4
In the embodiment, a mixed solution prepared from sodium cyanide, potassium ferricyanide, potassium thiocyanate, sodium nitrite and sodium sulfide is used as a measurement water sample, wherein the concentration of cyanide ions is 15.0mg/L, the concentration of ferricyanide compounds (calculated by cyanide) is 100.0mg/L, the concentration of nitrite is 20.0mg/L, the concentration of thiocyanate is 500mg/L and the concentration of sodium sulfide is 500mg/L. The concentration of cyanide ions in the above water sample was measured by the measurement method of example 1, which differs from example 1 only in that: in the step S1, 100mL of water sample is added with water to dilute to 200mL of solution to be tested, other steps are basically the same as those of the embodiment 1, and are not repeated herein, in the testing process, deionized water is used for blank test, four groups of cyanide ions are tested in parallel, the concentrations of the cyanide ions are respectively 14.4mg/L, 14.7mg/L, 14.8mg/L and 14.6mg/L, the recovery rate of the cyanide ions is 96.0-98.7%, partial cyanide ions are generated in the water sample in view of the composition characteristics of the water sample, the testing result is higher, and the effect of other interference ions such as nitrite ions, sulfur ions and the like can be eliminated by the testing method provided by the invention, so that the concentration of the cyanide ions in the water sample to be tested can be accurately tested.
In summary, according to the method for determining cyanide ions in complex water quality provided by the invention, ascorbic acid is added into a diluent of a water sample to be tested under the water bath condition of 50-70 ℃, so that possible oxidizing substances in the water quality are eliminated, nitrogen is introduced to blow off cyanide ions in the form of HCN, the blown-off HCN passes through lead acetate cotton, the blown-off HCN is absorbed by using sodium hydroxide absorption liquid, and then rhodanine is used as an indicator, and the content of cyanide ions in the water sample to be tested can be accurately determined by titration by using silver nitrate solution. In the process, the free cyanide ions are removed from the water sample in the form of HCN, and then analysis and determination are carried out, so that the influence of interfering ions or substances in the water sample on the cyanide ions is effectively eliminated, and the accuracy of determining the cyanide ions is improved. In addition, the method can accurately measure the cyanide ion concentration in complex water such as cyanide backwater, barren liquor and the like, provides an effective metering mode for the addition of sodium cyanide in the gold extraction process in the gold industry, and has important significance on environmental protection and carbon emission.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The method for determining cyanide ions in complex water quality, which is cyanide backwater and barren solution in cyanide gold extraction process, is characterized by comprising the following steps:
s1, taking a proper amount of water sample into a reaction bottle, adding water to dilute the water sample to 200mL, adding ascorbic acid and phenolphthalein solution under the water bath condition, and regulating the solution to be alkaline by using a first sodium hydroxide solution; then, connecting a pipeline, enabling the outlet end of the air duct to be inserted into sodium hydroxide absorption liquid, adding concentrated phosphoric acid into the reaction bottle, rapidly introducing nitrogen into the reaction bottle, and adjusting the flow of the nitrogen to enable cyanide ions to be blown off in a HCN mode;
s2, transferring the sodium hydroxide absorption liquid with HCN absorbed in the step S1 into a distillation flask, adding a second sodium hydroxide solution, stannous chloride solution, copper sulfate solution and the concentrated phosphoric acid, absorbing the distillate by using a third sodium hydroxide solution with the concentration of 2%, distilling to 100mL, and stopping heating;
s3, after the distillate obtained in the step S2 is subjected to distillation treatment to a constant volume, titrating with a silver nitrate solution by taking rhodanine as an indicator, and calculating the cyanide ion content.
2. The method for measuring cyanide ions in complex water according to claim 1, wherein in step S1, lead acetate cotton is placed in an air duct at the front end of the sodium hydroxide absorption liquid.
3. The method for measuring cyanide ions in complex water according to claim 1, wherein in step S1, the temperature range of the water bath condition is 50 to 70 ℃.
4. The method for measuring cyanide ions in complex water according to claim 1, wherein in the step S2, the mass concentration of the second sodium hydroxide solution is 100g/L, and the addition amount is 3.0mL; the concentration of the stannous chloride solution is 50g/L, and the adding amount is 2.0mL; the concentration of the copper sulfate solution is 200g/L, and the addition amount is 10mL; the addition amount of the concentrated phosphoric acid is 10mL.
5. The method for measuring cyanide ions in complex water according to claim 1, wherein in the step S2, the nitrogen gas is blown at a speed of 350 to 500ml/min, the purity of the nitrogen gas is 99.99%, and the blowing time is 30min.
6. The method for measuring cyanide ions in complex water according to claim 1, wherein in the step S1, the concentration of the ascorbic acid is 1%, and the addition amount is 5.0mL.
7. The method for determining cyanide ions in complex water according to claim 2, wherein in step S1, the lead acetate cotton is prepared by the following steps: 10g of lead acetate is dissolved in 100mL of water to obtain a lead acetate solution, and 10g of absorbent cotton is soaked in the lead acetate solution and taken out for airing.
8. The method for measuring cyanide ions in complex water according to claim 1, wherein in step S1, the concentration of the sodium hydroxide absorption liquid is 5.0g/L.
9. The method for measuring cyanide ions in complex water according to claim 1, wherein in the step S1, the amount of the concentrated phosphoric acid added is 10mL.
10. The method for measuring cyanide ions in complex water according to claim 1, wherein in the step S3, the concentration of the silver nitrate solution is 0.0100mol/L.
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| CN102773494A (en) * | 2011-05-13 | 2012-11-14 | 华东理工大学 | Method for preparing silver-coated copper powder through radiation reduction |
| CN104833674A (en) * | 2015-05-13 | 2015-08-12 | 长春黄金研究院 | Measuring method for cyanides in cyanide-containing wastewater of gold mine |
| 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 |
| 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 |
| 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 |
| 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 |
| CN108303492B (en) * | 2018-01-21 | 2020-06-26 | 长春黄金研究院有限公司 | Method for determining cyanide easily released in cyanide-containing solid waste containing sulfide |
| CN111257494B (en) * | 2020-01-13 | 2022-08-19 | 南京市产品质量监督检验院 | Method for detecting cyanide content in gold product by electroforming process through headspace gas chromatography |
| CN112285270A (en) * | 2020-09-07 | 2021-01-29 | 长春黄金研究院有限公司 | Method for determining total cyanide in water containing hydrogen peroxide |
| CN113030071A (en) * | 2021-02-22 | 2021-06-25 | 长春黄金研究院有限公司 | Method for determining cyanide easily released in thiocyanate-containing water |
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