CN106501218B - A kind of measuring method and device of carbon disulfide - Google Patents
A kind of measuring method and device of carbon disulfide Download PDFInfo
- Publication number
- CN106501218B CN106501218B CN201610970159.5A CN201610970159A CN106501218B CN 106501218 B CN106501218 B CN 106501218B CN 201610970159 A CN201610970159 A CN 201610970159A CN 106501218 B CN106501218 B CN 106501218B
- Authority
- CN
- China
- Prior art keywords
- solution
- carbon disulfide
- gas
- diethylamine
- diaphragm plate
- 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.)
- Expired - Fee Related
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/47—Scattering, i.e. diffuse reflection
- G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
- G01N21/51—Scattering, i.e. diffuse reflection within a body or fluid inside a container, e.g. in an ampoule
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Present invention discloses a kind of measuring method of carbon disulfide and devices, it is to absorb the excessive alkaline ethylenediamine solution of carbon disulfide, so that carbon disulfide and alkali and diethylamine is reacted and generates deliquescent ethylenediamine dithio formate product, ethylenediamine dithio formate product in absorbing liquid mixes the generation that reacts with acid solution (or element in acid solution) again has volatile volatile matter, by carrying out Quick gas-liquid separation to the solution containing volatile matter, the escaping gas isolated is set to pass through light scattering method (or atomic spectroscopy) to measure the concentration of carbon disulfide.It also discloses simultaneously and carries out carbon disulfide measurement device, when mainly mixed solution above diaphragm plate by flowing through, solution above is bubbled by leading to carrier gas below diaphragm plate, to carry out gas-liquid separation.Preparation of the volatile matter isolated for atom spectrum gaseous state sample introduction or chemical vapor deposition precursor.
Description
Technical field
The invention belongs to the measuring methods and device of environmental science more particularly to a kind of carbon disulfide.
Background technique
Carbon disulfide is colourless or yellow effumability toxic liquid, can manufacture viscose rayon, four atmosphere carbon, promote
The products such as agent is also a kind of widely used organic solvent, its boiling point is lower (4 3 DEG C of .6), inflammable and explosive (quick-fried
The fried limit: 1 .2 5% of lower bound, 44 % of high limit).Carbon disulfide gas through respiratory tract invade human body after, can make one headache,
Dizziness, general weakness, vision and sensory disturbance, digestive disorders serious person will cause refreshing smart system disorders.Therefore, Accurate Determining
Carbon disulfide is of great significance
The method for being usually used in measuring carbon disulfide at present has gas chromatography and absorption photometry.The former operate it is cumbersome,
The latter's sensitivity is low, and there are H2The interference such as S, cannot meet the requirement of micro-analysis in environmental sample well.The latter's result
It is unstable, and detection limit is poor.
Currently, the present inventor is under study for action, by being acidified sodium diethyldithiocarbamate online, then quick separating
It is very strong light scattering to find that volatile matter has for the volatile matter of generation, therefore the present inventor proposes a kind of survey of carbon disulfide with regard to this
Determine method and apparatus, thereby completing the present invention.
Summary of the invention
The present invention discloses a kind of measuring method of carbon disulfide first, it is characterised in that by the excessive alkali of carbon disulfide
Property diethylamine solution absorb, so that alkali and carbon disulfide and diethylamine is reacted and generate diethyldithiocarbamate.It inhales
Diethyldithiocarbamate in liquid is received again with acid solution or the acid solution containing element mixes to react makes two
Diethyldithiocar bamic acid salt generates the diethyldithiocar bamic acid with volatile light scatter properties, or generates tool
There is volatile diethyldithiocar bamic acid element complex, by carrying out Quick gas-liquid separation to solution, makes to isolate
Diethyldithiocar bamic acid gas or diethyldithiocar bamic acid element complex pass through light scattering method or atom
Spectroscopic methodology measures the concentration of carbon disulfide.
Absorbing liquid used in the present invention refers to the diethylamine solution of alkalinity, refers to the alkaline solution that pH is greater than 7.It is preferred that pH
Value greater than 10 alkali metal potassium, sodium, the hydroxide solution of lithium (or alkaline earth metals calcium, magnesium, strontium) and diethylamine mixed solution.
Wherein the content of hydroxide and the content of diethylamine are excessive for carbon disulfide to be determined.
In the present invention, the solution after reacting is reacted to by gas-liquid separation from absorbing liquid in line and acid solution, when total
Between less than 10 seconds, preferably smaller than 5 seconds.
In the present invention, the acidity of absorbing liquid solution after line is mixed with acid solution is 0.01 between 0.1M, is preferably inhaled
The acidity for receiving liquid solution after line is mixed with acid solution is 0.012 between 0.05M.
In the present invention, when determination of volatile matter, light scattering method excitation wavelength used was the preferred excitation wave of 190nm -800nm.
A length of 190nm -280nm.
As a particularly suitable instrument, an atomic fluorescence of zero dispersion photometer is selected to cooperate the gas in the present invention again
Liquid separating apparatus, it is easy to realize measurement of the invention.
It is then by the way that excessive diethylamine and hydroxide is added to aqueous solution to be measured when the sample of measurement is aqueous solution
To prepare testing sample solution.
In the present invention, when measuring the concentration of carbon disulfide using atomic spectroscopy, at this time also containing solid in acid solution
Quantitative metal ion.Its principle is that carbon disulfide and diethylamine and metal ion can generate volatile gold in acid condition
Belong to complex compound.When two sulphur in metal ion one timing of content in an acidic solution, the concentration and solution of the metal volatile matter of generation
It is linear to change concentration of carbon.The atom spectrum intensity of metal thus can be measured to measure the content of carbon disulfide.Use this
When method, the metal ion preferably (but being not limited to) content is in the zinc of 5-100ppb, cadmium, nickel, cobalt, iron, manganese and chromium.
The present invention also proposes the device for carbon disulfide measurement, is characterized in that the device includes acid solution or containing element
Acid solution ingress pipe (1), diethyldithiocarbamate solution containing carbon disulfide ingress pipe 2, peristaltic pump 3,
3 ', 4 gas-liquid separator 5 of tee tube, carrier gas inlet 6, carrier gas outlet 7 and discharging of waste liquid pipe 8；First peristaltic pump 3 passes through threeway 4
It is connected with gas-liquid separator 5, it is 25-50 centimetres that gas-liquid separator 5, which has a diameter close to the place of bottom, aperture 50-150 mesh is more
The permeable watertight diaphragm plate 9 in hole, the porous permeable watertight diaphragm plate diameter of gas-liquid separator is preferably 30-40 centimetres, diaphragm plate hole
Diameter is preferably 70-90 mesh.Discharging of waste liquid pipe 8, discharging of waste liquid pipe and second wriggling are connected on the diaphragm plate of permeable watertight
(3 ') are pumped to be connected.When mixed solution above diaphragm plate by flowing through, solution above is bubbled by leading to carrier gas below diaphragm plate,
To carry out gas-liquid separation.
Acid solution (or acidity containing element) sample solution ingress pipe 1, the diethyl-dithio amino containing carbon disulfide
The flow velocity of the ingress pipe 2 of formates (M-DDTC) solution is 1.0-3.0 ml/min.It is preferred that 1.5-2.5 ml/min.
The solution of diethyldithiocarbamate (M-DDTC) on the device and Element Solution on-line mixing to be measured
And the gas-liquid separation time amounted to less than 10 seconds.
The solution of diethyldithiocarbamate (M-DDTC) and Element Solution on-line mixing to be measured and gas-liquid separation
Time amounted to less than 5 seconds.
Mixed solution acidity on the device is 0.0125-0.2 mol/L.
The present invention focuses on carbon disulfide to react generation diethyl-dithio amino first with diethylamine and alkali hydroxide
After hydrochlorate, diethyldithiocar bamic acid or diethyldithiocar bamic acid-that product generates in acid condition
The volatility of metal complex.It is studied by this, spy solves curing Carbon analysis problem, a kind of curing especially set out
Carbon analysis method.
Possessed good effect exists the measuring method and device of carbon disulfide disclosed by the invention compared with prior art
In:
(1) finding speed is fast, as long as by be measured containing the diethyldithiocar bamic acid of carbon disulfide or its Yu Yuansu
Then alkaline aqueous solution and the acid solution mixing of formation carry out gas-liquid separation, instrument can determine the content of carbon disulfide.No
As gas-chromatography and colorimetric spectrophotometer, the pretreatment process that needs to grow very much.
(2) detection limit is good, between the detection limit 0.05ppm of carbon disulfide that the present invention is measured is arrived.Better than existing point
Photolorimetry.
(3) without any interference.Whether muddy solution or coloured solution, this method can measure.And it is divided
Rule cannot measure colored solutions.Especially by the interference of hydrogen sulfide.
Detailed description of the invention
Fig. 1 is the device figure for being suitable for the invention sample introduction；Wherein:
1, acid solution or the acid solution ingress pipe containing element
2, the diethyldithiocarbamate solution ingress pipe containing carbon disulfide
3, the first peristaltic pump, 3 ' second peristaltic pumps
4, tee tube
5, gas-liquid separator
6, carrier gas inlet
7, carrier gas exports
8, discharging of waste liquid pipe
9, the porous permeable watertight diaphragm plate of aperture 50-150 mesh.
Specific embodiment
In order to more fully explain implementation of the invention, provides and following of the invention prepare embodiment.These implement real
Example is only to explain, be not intended to limit the scope of the invention.
Embodiment 1
(1) 50 liters of certain workplace gaseous sample is adopted with gas sampler, makes the carbon disulfide in gaseous sample by excess
Sodium hydroxide (pH=13) and diethylamine (40mM) mixed solution absorb, then, use peristaltic pump with the stream of 1.2 ml/mins
Speed extracts above-mentioned absorbent solution, while extracting the hydrochloric acid solution that an acidity is 0.2 M with certain flow rate, adjusts sour sample feeding pipe stream
Amount makes the final acidity of two mixed solutions make two strands of 1 sampling devices of solution by specification attached drawing in a tee tube in 0.05M.
In converge after react.
(2) by the solution after the volatile matter of generation and reaction, gas-liquid separator is carried out in 1 sampling device of Figure of description
Separation；
(3) the DDTC acid volatile matter isolated is imported into an atomic fluorescence of zero dispersion photometer and carries out the scattered color measurement of light
(with the hollow cathode lamp most excitation light source of zinc), after carbon disulfide scattering strength and standard carbon disulfide are dissipated intensity of colour comparison,
Obtaining content in atmosphere is 20ppm.This measured value and spectrophotometry measured value have coincide well.
Embodiment 2
(1) (make mixed hydrogen to excessive sodium hydroxide and diethylamine is added in certain 100 milliliters of aqueous sample to be measured
Aoxidize na concn 0.15M, diethylamine 100mM), then, peristaltic pump is used to extract above-mentioned absorption with the flow velocity of 1.7 ml/mins
Solution, while two strands of solution are made illustratively with the nitric acid solution that same flow velocity extracts the 20ppb containing zinc that an acidity is 0.2 M
1 sampling device of book attached drawing reacts after converging in a tee tube.
(2) by the solution after the volatile matter of generation and reaction, gas-liquid separator is carried out in 1 sampling device of Figure of description
Separation；
(3) DDTC-zinc volatile matter isolated is imported into an atomic fluorescence of zero dispersion photometer and carries out atomic fluorescence
Measurement measurement is solved the fluorescence intensity of zinc and the linear relationship of vulcanization concentration of carbon by experiment, obtains and contain in waste water carbon disulfide
Amount is 5ppm.This measured value and spectrophotometry measured value have coincide well.
A kind of device formed for element evaporation object,
The device includes acid (or acidity containing element) solution ingress pipe 1, the diethyl-dithio ammonia containing carbon disulfide
Ingress pipe 2, peristaltic pump 3,3 ', 4 gas-liquid separator 5 of tee tube, carrier gas inlet 6, carrier gas outlet 7 and the waste liquid of base formate solution
Delivery pipe 8；First peristaltic pump 3 is connected by threeway 4 with gas-liquid separator 5, and gas-liquid separator 5 has one close to the place of bottom
Diameter is 30 centimetres, the porous permeable watertight diaphragm plate 9 of 80 mesh of aperture, when mixed solution above diaphragm plate by flowing through, by film
Lead to carrier gas below plate to be bubbled solution above, to carry out gas-liquid separation.
The wherein acid solution on the device (or acid solution containing element) ingress pipe (1), the diethyl containing carbon disulfide
The flow velocity of the ingress pipe (2) of base dithiocar-bamate ((M-DDTC)) solution is 1.0-2.5 ml/min, preferably 1.5-
2.0 ml/mins, the at this time preferred 1:1 of the ratio of two flow velocitys.
The solution of diethyldithiocarbamate (M-DDTC) on the device and acid solution on-line mixing to be measured
And the gas-liquid separation time amounted to less than 10 seconds.
The solution of diethyldithiocarbamate (M-DDTC) with when acid solution on-line mixing and gas-liquid separation
Between amount to less than 5 seconds.
Mixed solution acidity on the device is 0.0125-0.2 mol/L.
Embodiment 4
Comparative test
Conclusion:
(1) finding speed of the present invention is fast
(2) it is not interfered by sample solution color.Especially not by the interference of hydrogen sulfide.
(3) detection limit is low, better than existing method at present.
After the preferred embodiment of detailed description, it is familiar with this skilled worker and is clearly understood that, it is above-mentioned not departing from
Various change and modification can be carried out under claim and spirit, it is all according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent change and modification of work belong to the range of technical solution of the present invention.
Claims (1)
1. a kind of measuring method of carbon disulfide, it is characterised in that the excessive alkaline diethylamine solution of carbon disulfide is absorbed,
Carbon disulfide and alkaline diethylamine is set to react and generate deliquescent diethyl-dithio formates product, two in absorbing liquid
Ethyl dithio formate product again with hydrochloric acid solution or the nitric acid solution on-line mixing containing zinc react generation have volatilization
Property volatile matter, by containing volatile matter solution carry out Quick gas-liquid separation, so that the escaping gas isolated is passed through light
Scattering method or atomic spectroscopy measure the concentration of carbon disulfide；Gas-liquid separator (5) has the diameter to be close to the place of bottom
25-50 centimetres, the porous permeable watertight diaphragm plate (9) of aperture 50-150 mesh, when mixed solution above diaphragm plate by flowing through, by
Lead to carrier gas below diaphragm plate to be bubbled solution above, to carry out gas-liquid separation；On-line mixing and gas-liquid separation time are total
Meter was less than 10 seconds；
The alkaline diethylamine solution is the hydroxide solution and diethylamine of alkali metal of the pH value greater than 10, alkaline-earth metal
Mixed solution；The alkali metal is potassium, sodium, lithium；Alkaline-earth metal refers to calcium, magnesium, strontium；
The acidity of absorbing liquid solution after line is mixed with acid solution is 0.01 between 0.1M；
The light scattering method refers to: light scattering method excitation wavelength is 190nm -800nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610970159.5A CN106501218B (en) | 2016-11-07 | 2016-11-07 | A kind of measuring method and device of carbon disulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610970159.5A CN106501218B (en) | 2016-11-07 | 2016-11-07 | A kind of measuring method and device of carbon disulfide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106501218A CN106501218A (en) | 2017-03-15 |
| CN106501218B true CN106501218B (en) | 2019-10-15 |
Family
ID=58322838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610970159.5A Expired - Fee Related CN106501218B (en) | 2016-11-07 | 2016-11-07 | A kind of measuring method and device of carbon disulfide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106501218B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110806384A (en) * | 2019-12-06 | 2020-02-18 | 天津师范大学 | Sample introduction device of analytical instrument and use method |
| CN111551511A (en) * | 2020-06-04 | 2020-08-18 | 江苏康达检测技术股份有限公司 | Spectrophotometry for measuring content of carbon disulfide in air |
| CN114689715B (en) * | 2020-12-29 | 2024-01-16 | 北京海浈医药科技有限公司 | Method for detecting trimethylamine or trimethylamine salt content |
-
2016
- 2016-11-07 CN CN201610970159.5A patent/CN106501218B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 金属-二乙基二硫代氨基甲酸螯合物的气相色谱研究(Ⅰ)螯合物的热分析和气相色谱;胡继明 等;《武汉大学学报（自然科学版）》;19821231(第4期);第47-54页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106501218A (en) | 2017-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106501218B (en) | A kind of measuring method and device of carbon disulfide | |
| CN107478734A (en) | The chromatography of ions detection method of sulfate radical and inferior sulfate radical is determined in a kind of desulfurization seawater simultaneously | |
| Moss et al. | Determination of textra-alkyl lead vapour and inorganic lead dust in air | |
| CN106645371A (en) | Determination method for heavy metal content in mineral water | |
| CN103323412A (en) | Thiocyanate spectrophotometry method for detecting iron content of high-temperature alloy | |
| CN106645056B (en) | A kind of detection method of barium in drinking water ion | |
| CN108303492B (en) | Method for determining cyanide easily released in cyanide-containing solid waste containing sulfide | |
| CN109633079A (en) | A method of vanadium and ammonium content in detection metavanadate solution | |
| Jaikang et al. | Conductometric determination of ammonium ion with a mobile drop | |
| CN109470813A (en) | The measuring method of chlorine and bromine content in plastics | |
| CN107991429A (en) | The assay method of cyanide is easily discharged in a kind of cyanide wastewater of sulfur compound | |
| CN103630601A (en) | Determination method for specific migration quantities of multiple elements in cigarette filter | |
| CN104849400A (en) | Novel method for measuring content of zinc in alkaline zinc-nickel alloy plating solution | |
| CN102944551B (en) | A kind of Cd 2+detection method | |
| CN103487391A (en) | Testing method for lead content in water body | |
| CN103234957B (en) | Method for determining concentration of cyanides in environment | |
| Afkhami et al. | Indirect determination of sulfide by cold vapor atomic absorption spectrometry | |
| CN106483157A (en) | The determination method of total chlorine in a kind of doctor solution | |
| CN111189956A (en) | By means of H2O2Method for detecting content of nitrite in sodium chloride sample by combining oxidation method with ion chromatography | |
| Škrlíková et al. | An air-assisted liquid–liquid extraction using a dual-valve sequential injection manifold (DV-SIA): Determination of copper | |
| CN206515230U (en) | It is a kind of at the same measure air in nitrous acid, ozone, the equipment of nitrogen dioxide | |
| Sritharathikhun et al. | On-line collection/concentration and detection of sulfur dioxide in air by flow-injection spectrophotometry coupled with a chromatomembrane cell | |
| Okumura et al. | A simple and rapid in situ preconcentration method using solid-phase extraction for the determination of dissolved Manganese in brackish lake water samples | |
| CN108956595A (en) | A kind of reagent of the quick colorimetric detection ammonium root of high stable | |
| Morosanova et al. | Length-of-stain indicator tubes for the determination of metals in water and solutions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20191015 Termination date: 20201107 |