CN109374608A - A kind of method of spectrophotometry amine collector - Google Patents
A kind of method of spectrophotometry amine collector Download PDFInfo
- Publication number
- CN109374608A CN109374608A CN201811226293.XA CN201811226293A CN109374608A CN 109374608 A CN109374608 A CN 109374608A CN 201811226293 A CN201811226293 A CN 201811226293A CN 109374608 A CN109374608 A CN 109374608A
- Authority
- CN
- China
- Prior art keywords
- solution
- amine
- absorbance
- measured
- concentration
- 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.)
- Granted
Links
- 150000001412 amines Chemical class 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002798 spectrophotometry method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 238000005259 measurement Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 49
- 238000002835 absorbance Methods 0.000 claims description 33
- 239000011259 mixed solution Substances 0.000 claims description 28
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000011088 calibration curve Methods 0.000 claims description 16
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical group CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 14
- 150000003141 primary amines Chemical class 0.000 claims description 5
- 150000001768 cations Chemical class 0.000 claims description 4
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 2
- 241000208340 Araliaceae Species 0.000 claims 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- AJXBTRZGLDTSST-UHFFFAOYSA-N amino 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON AJXBTRZGLDTSST-UHFFFAOYSA-N 0.000 claims 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000002474 experimental method Methods 0.000 abstract description 5
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000004587 chromatography analysis Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- 238000000605 extraction Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
A kind of method of amine collector in spectrophotometry water quality, is related to chemistry, floating agent/environmental test determination techniques field, and the method for the present invention includes amine collector concentration in the production method of amine collector standard curve and measurement sample to be tested.Relative to bromophenol blue spectrophotometry, gold orange II spectrophotometry and liquid (gas) phase chromatography, the method of the present invention simplifies detecting step, cost needed for color developing agent used in experiment greatly reduces harm and experiment in experimentation to operator and environment, pass through condition optimizing simultaneously, make this method that there is good reliability, wider detection range.
Description
Technical field
The present invention relates to chemistry, floating agent and environmental test determination techniques fields, and in particular to a kind of spectrophotometry
The method for detecting amine collector.
Background technique
Amine collector is widely used in silicate, carbonate and solubility salt Mineral Floating Process, but amine is caught
Receiving agent is a kind of bio-refractory and highly toxic organic compound, and serious pollution can be caused to water body environment.However at present
It is less to the relevant report of amine collector concentration mensuration and discharge standard in water quality both at home and abroad, and there are some problems.Often
The measurement and liquid chromatograph or gas chromatograph combination that quantitative analysis method is TOC (total organic carbon), but TOC detector
And chromatograph price is more expensive.There is document to mention using bromophenol blue or gold orange II complexing amine collector, and uses three chloromethanes
The spectrophotometric method of alkane extraction measures its concentration, this method high sensitivity, but artificial complexing and extraction process are cumbersome, and extraction is not
Completely, and chloroform is light sensitive, meets phosgene and hydrogen chloride that photodegradation generates severe toxicity, can make to operator and environment
At harm.
Therefore, it is necessary to a kind of new methods for measuring amine collector spectrophotometric, can mitigate due to using chloroform
The caused harm to human body, and sensitivity, accuracy in detection process can not be reduced.
Summary of the invention
The present invention provides a kind of method of spectrophotometry amine collector, technical problem to be solved is
Detection amine collector spectrophotometric new system is established, has selected a kind of new color developing agent Congo red to substitute in old system
Bromophenol blue or gold orange II, and the extraction of chloroform is omitted, simplify experimental implementation, while reducing chloroform to personnel and ring
It is endangered caused by border.This method can provide technical foundation for the water quality of amine collector from now on/mine environmental influence research.
For the present invention using the concentration of amine collector in water by Spectrophotometry matter, design is added into sample to be tested
Enter hac buffer and adjust pH value of solution=5, shake up, Congo red progress complex reaction is added and develops the color, after standing 10min, uses
10mm cuvette carries out colorimetric at wavelength 497nm.
A kind of method of spectrophotometry amine collector is carried out according to following steps:
1. amine collector concentration is abscissa x using absorbance as ordinate y, calibration curve equation, the extinction are established
Degree is that amine collector, hac buffer and Congo red solution mixed solution absorbance subtract and reference deionized water absorbance
Value；
2. it is 5 that sample to be tested, which is added hac buffer to adjust pH value of solution, it is 5 × 10 that concentration, which is added,-4The Congo of mol/L
Red solution is uniformly mixed with deionized water constant volume, stands 10 minutes, obtains mixed solution to be measured, the sample to be tested, Congo red
The volume ratio of solution and mixed solution to be measured be 5:2:25, by mixed solution to be measured be placed in ultraviolet specrophotometer wavelength 490~
Absorbance is measured at 497nm；
3. it is subtracted using mixed solution absorbance to be measured as the value of the deionized water absorbance of reference as ordinate y value,
Substitute into step 1. described in calibration curve equation, the concentration of amine collector in sample to be tested is calculated.
Preferably, the volume ratio of the sample to be tested, hac buffer, Congo red solution and mixed solution to be measured is 5:
1:2:25。
Preferably, the establishment process of the calibration curve equation is as follows:
The amine collector solution of at least five kinds of various concentrations is prepared, selected concentration is in 0.00~20.00mg/L range
It is interior；Being separately added into hac buffer makes pH value of solution=5, with 5 × 10-4The Congo red solution of mol/L is color developing agent, and mixing is equal
It is even, 10 minutes are stood, mixed solution is obtained；The volume ratio of the amine collector solution, Congo red solution and mixed solution to be measured
For 5:2:25；Mixed solution to be measured is placed in measurement absorbance at 490~497nm of ultraviolet specrophotometer wavelength, with deionization
Water is reference measurement absorbance, subtracts the deionized water absorbance as reference as ordinate y using mixed solution absorbance to be measured,
Using amine collector concentration as abscissa x, curve is drawn, calibration curve equation is obtained.
Preferably, the establishment process of the calibration curve equation is as follows:
The amine collector solution of at least five kinds of various concentrations is prepared, selected concentration is in 0.00~20.00mg/L range；
Being separately added into hac buffer makes pH value of solution=5, with 5 × 10-4The Congo red solution of mol/L is color developing agent, is uniformly mixed, quiet
It sets 10 minutes, obtains mixed solution；The volume ratio of the amine collector solution, Congo red solution and mixed solution to be measured is 5:2:
25；Mixed solution to be measured is placed in measurement absorbance at ultraviolet specrophotometer wavelength 497nm, using deionized water as reference measurement
Absorbance subtracts the deionized water absorbance as reference as ordinate y, with amine collector using mixed solution absorbance to be measured
Concentration is abscissa x, draws curve, obtains calibration curve equation.
Preferably, the volume of the amine collector solution, hac buffer, Congo red solution and mixed solution to be measured
Than for 5:1:2:25.
Preferably, the amine collector solution concentration is chosen within the scope of 0.00~20.00mg/L, selected concentration
It is worth evenly dispersed.
Further, the selection amine collector solution concentration is within the scope of 0.00~20.00mg/L, it is preferable that choosing
The concentration in gradient variation taken, the point of selection should not be concentrated.
Preferably, the establishment process of the calibration curve equation is as follows:
1. by 0.00,4.00,8.00,10.00,14.00,20.00mg/L amine collector solution is separately added into 1mL
Above-mentioned 6 solution examples are adjusted to pH=5 by hac buffer；
2. by step, 1. each solution of gained is separately added into the 5 × 10 of 2mL-4The Congo red solution of mol/L, deionized water are settled to
25mL is uniformly mixed, and is stood 10 minutes, is obtained mixed solution；
3. taking step, 2. acquired solution is statically placed in 10mm cuvette, at ultraviolet specrophotometer 497nm wavelength, to go
Ionized water is reference measurement absorbance；
4. subtracting the absorbance A of deionized water reference with the mixed solution absorbance A of measurement0For ordinate y, caught with amine
Receipts agent concentration is abscissa x, draws curve, obtains calibration curve equation.
Preferably, the calibration curve equation is y=-0.01577x+0.72964, R2=0.9906.
Preferably, the curve has linear relationship, R2> 0.99, detect amine collector concentration range be 0.8~
20mg/L。
Preferably, the amine collector uses primary amine cation-collecting agent or quaternaries cation collecting agent.
Preferably, the primary amine cation-collecting agent is lauryl amine or cetylamine collecting agent.
Preferably, the quaternaries cation collecting agent is dodecyl trimethyl ammonium chloride or trimethyl
Ammonium bromide collecting agent.
Compared with the method that technical background is previously mentioned, this method beneficial effect is: having selected a kind of new color developing agent rigid
Arnotto substitutes the bromophenol blue or gold orange II in old system, and the extraction of chloroform is omitted, and simplifies experimental implementation, drops simultaneously
Low chloroform is endangered caused by personnel and environment.This method can be amine collector water quality/mine environmental influence from now on
Research provides technical foundation.
Detailed description of the invention
Fig. 1 is the lauryl amine canonical plotting measured in the present invention.
Fig. 2 is the dodecyl trimethyl ammonium chloride canonical plotting measured in the present invention.
Fig. 3 is influence of the difference pH to chromogenic reaction absorbance in the present invention.
Fig. 4 is influence of the medium wavelength of the present invention to Congo red color developing agent absorbance.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Test agents useful for same is that analysis is pure, and test water is deionized water.
Embodiment 1
1, the preparation of solution:
Concentration is 5 × 10-4The Congo red solution of mol/L: it is Congo red to weigh 0.3483g, is dissolved in a small amount of water, is diluted to
1000mL is stored in brown bottle；
Lauryl amine solution: accurately weighing 0.0200g lauryl amine, and 3 drop hydrochloric acid are added dropwise, and is diluted with water to 1000mL and obtains concentration and is
20.00mg/L lauryl amine solution, being diluted with water and making concentration is 4.00mg/L, 8.00mg/L, 10.00mg/L, 14.00mg/L
Lauryl amine solution.
The hac buffer of pH=5: weighing 11.50g sodium acetate, and 1.4mL glacial acetic acid is added, and is diluted with water to
250mL, it is ready-to-use suitably with glacial acetic acid adjusting pH value of solution to 5.
2, the preparation of lauryl amine standard curve:
Respectively by 0.00,4.00,8.00,10.00,14.00,20.00mL/g lauryl amine collecting agent solution, each 5ml is added
6 25mL color-comparison tubes are added the hac buffer of 1mL pH=5, above-mentioned 6 samples are adjusted to pH=5；It is separately added into
The 5 × 10 of 2mL-4The Congo red solution of mol/L, is settled to 25mL, mixes, and stands 10 minutes；It is placed in 10mm cuvette, in
At 497nm wavelength, using deionized water as reference measurement absorbance；The extinction of deionized water reference is subtracted with the absorbance A of measurement
Spend A0Curve is drawn using lauryl amine collecting agent concentration in the serial solution of preparation as abscissa x for ordinate y, obtains standard song
Line equation: y=-0.01577x+0.72964, R2=0.9906, as shown in Fig. 1.
3, the concentration of lauryl amine collecting agent in water sample to be measured is measured:
It takes 5mL sample to be tested into 25mL colorimetric cylinder, measures sample absorbance A, lauryl amine in sample according to above-mentioned steps
The calculation formula of concentration are as follows:
ρ (mg/L)=(A-A0-0.72964)/(-0.01577)；
4, veracity and precision measurement experiment
The method in embodiment 1 is used to carry out 7 measurements to concentration for the lauryl amine of 10.00mg/L and 15.00mg/L,
The average value of 7 measurements is respectively 10.25mg/L and 15.10mg/L, and relative error is respectively 2.44% and 0.66%, opposite mark
Quasi- deviation (RSD) is respectively 3.69% and 4.10%, and this method accuracy, precision are good.
The analysis of 1 lauryl amine relative standard deviation of table
| Measurement result | 1 | 2 | 3 | 4 | 5 | 6 | 7 | Average value | RSD/% |
| 10.00mg/L | 10.23 | 10.56 | 10.83 | 10.50 | 10.26 | 10.06 | 9.28 | 10.25 | 3.69 |
| 15.00mg/L | 14.34 | 14.76 | 14.92 | 14.57 | 15.91 | 15.34 | 15.86 | 15.1 | 4.10 |
Embodiment 2
The calibration curve equation of primary amine and quaternary ammonium salt collecting agent.
The preparation of collecting agent solution: taking cetylamine collecting agent 0.0200g in 50 DEG C of deionized water, and the three dense salt of drop are added dropwise
Acid dissolution is placed in ultrasonator and is diluted to 1000mL with deionized water；0.0200g quaternary ammonium salt collecting agent (ten is taken respectively
Dialkyl group trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide) with dissolved in deionized water, be then diluted with water to 1000mL
Obtaining concentration is 20.00mg/L collecting agent solution, is diluted to required concentration respectively, obtains 4.00,8.00,10.00,14.00mg/L is molten
Liquid.
According to the method for embodiment 1, other amine collector (cetylamine, dodecyl trimethyl ammonium chloride, 12 are tested
Alkyl trimethyl ammonium bromide) calibration curve equation, enumerate the standard curve of dodecyl trimethyl ammonium chloride (quaternary ammonium salt)
As shown in Figure 2.The coefficient R of the resulting standard curve of serial solution2>0.99, relative deviation<5% of Duplicate Samples, result
Such as following table.Thus illustrate that the test method is suitable for the concentration mensuration of amine collector.
Other amine collector calibration curve equations of table 2
Implementation column 3
Analysis is sampled to tap water and Hun River surface water river, carries out recovery testu, measures amine in water body
As a result collecting agent concentration is listed in table 3.
3 environmental water sample measurement result of table
| Water sample | Additional amount (mg/L) | Total measured value (mg/L) | The rate of recovery/% |
| Tap water | 5 | 4.83 | 96.6 |
| Hun River water | 5 | 5.21 | 104.2 |
By above experiment sum number it was demonstrated that the method sensitivity of this experiment, accuracy are good, relative standard deviation compared with
Small, recovery of standard addition is high, with respect to the background art the method, this experimental implementation is simple, highly-safe, will not be to operator
It causes damages with environment.
Claims (9)
1. a kind of method of spectrophotometry amine collector, which is characterized in that carried out according to following steps:
1. amine collector concentration is abscissa x using absorbance as ordinate y, calibration curve equation is established, the absorbance is
Amine collector, hac buffer and Congo red solution mixed solution absorbance subtract and reference deionized water absorbance
Value；
2. it is 5 that sample to be tested, which is added hac buffer to adjust pH value of solution, it is 5 × 10 that concentration, which is added,-4Mol/L's is Congo red molten
Liquid is uniformly mixed with deionized water constant volume, is stood 10 minutes, is obtained mixed solution to be measured, the sample to be tested, Congo red solution
Volume ratio with mixed solution to be measured is 5:2:25, and mixed solution to be measured is placed in 490~497nm of ultraviolet specrophotometer wavelength
Place's measurement absorbance；
3. being subtracted using mixed solution absorbance to be measured as the value of the deionized water absorbance of reference as ordinate y value, substitute into
Step 1. described in calibration curve equation, the concentration of amine collector in sample to be tested is calculated.
2. the method according to claim 1, wherein the sample to be tested, hac buffer, Congo red solution
Volume ratio with mixed solution to be measured is 5:1:2:25.
3. the method according to claim 1, wherein the establishment process of the calibration curve equation is as follows:
The amine collector solution of at least five kinds of various concentrations is prepared, selected concentration is within the scope of 0.00~20.00mg/L；Point
Not Jia Ru hac buffer make pH value of solution=5, with 5 × 10-4The Congo red solution of mol/L is color developing agent, is uniformly mixed, and is stood
10 minutes, obtain mixed solution；The volume ratio of the amine collector solution, Congo red solution and mixed solution to be measured is 5:2:
25；Mixed solution to be measured is placed in measurement absorbance at 490~497nm of ultraviolet specrophotometer wavelength, is ginseng with deionized water
Than measuring absorbance, the deionized water absorbance as reference is subtracted as ordinate y, with amine using mixed solution absorbance to be measured
Collecting agent concentration is abscissa x, draws curve, obtains calibration curve equation.
4. according to the method described in claim 3, it is characterized in that, the amine collector solution, hac buffer, the Congo
The volume ratio of red solution and mixed solution to be measured is 5:1:2:25.
5. according to the method described in claim 3, it is characterized in that, the amine collector solution concentration 0.00~
It is chosen within the scope of 20.00mg/L, selected concentration value is evenly dispersed.
6. according to the method described in claim 3, it is characterized in that, the curve has linear relationship, R2> 0.99, detect amine
The concentration range of collecting agent is 0.8~20mg/L.
7. according to the method described in claim 3, it is characterized in that, the amine collector uses primary amine cation-collecting agent
Or quaternaries cation collecting agent.
8. the method according to the description of claim 7 is characterized in that the primary amine cation-collecting agent is lauryl amine or 16
Amine collecting agent.
9. the method according to the description of claim 7 is characterized in that the quaternaries cation collecting agent is dodecyl three
Ammonio methacrylate or dodecyl trimethyl ammonium bromide collecting agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811226293.XA CN109374608B (en) | 2018-10-18 | 2018-10-18 | Method for detecting amine collecting agent by spectrophotometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811226293.XA CN109374608B (en) | 2018-10-18 | 2018-10-18 | Method for detecting amine collecting agent by spectrophotometry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109374608A true CN109374608A (en) | 2019-02-22 |
| CN109374608B CN109374608B (en) | 2021-05-28 |
Family
ID=65400632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811226293.XA Active CN109374608B (en) | 2018-10-18 | 2018-10-18 | Method for detecting amine collecting agent by spectrophotometry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109374608B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112285044A (en) * | 2020-10-27 | 2021-01-29 | 北京大学 | Online differential ultraviolet-visible spectrum detector for organic matters in water and organic matter detection method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050037509A1 (en) * | 2003-08-13 | 2005-02-17 | Richard Geisler | Method for determining surfactant concentration in aqueous solutions |
| CN101825578A (en) * | 2010-04-16 | 2010-09-08 | 武汉理工大学 | Improved method for measuring concentration of amine cation-collecting agent |
| CN103575666A (en) * | 2012-07-26 | 2014-02-12 | 中国石油天然气股份有限公司 | Online photoelectric detection device and detection method for residual concentration of corrosion inhibitor |
| CN103861733A (en) * | 2014-03-26 | 2014-06-18 | 东北大学 | Method for preparing super iron concentrates through magnetic separation-reverse flotation technology |
| CN105074420A (en) * | 2013-03-15 | 2015-11-18 | 艾瑞思国际股份有限公司 | Hematology systems and methods |
| CN106802296A (en) * | 2015-12-02 | 2017-06-06 | 浙江闰土研究院有限公司 | A kind of method for quick of the extent of reaction of Dyestuff synthesis coupling reaction |
| JP2018024787A (en) * | 2016-08-10 | 2018-02-15 | 株式会社サクラクレパス | Colorable ink composition |
-
2018
- 2018-10-18 CN CN201811226293.XA patent/CN109374608B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050037509A1 (en) * | 2003-08-13 | 2005-02-17 | Richard Geisler | Method for determining surfactant concentration in aqueous solutions |
| CN101825578A (en) * | 2010-04-16 | 2010-09-08 | 武汉理工大学 | Improved method for measuring concentration of amine cation-collecting agent |
| CN103575666A (en) * | 2012-07-26 | 2014-02-12 | 中国石油天然气股份有限公司 | Online photoelectric detection device and detection method for residual concentration of corrosion inhibitor |
| CN105074420A (en) * | 2013-03-15 | 2015-11-18 | 艾瑞思国际股份有限公司 | Hematology systems and methods |
| CN103861733A (en) * | 2014-03-26 | 2014-06-18 | 东北大学 | Method for preparing super iron concentrates through magnetic separation-reverse flotation technology |
| CN106802296A (en) * | 2015-12-02 | 2017-06-06 | 浙江闰土研究院有限公司 | A kind of method for quick of the extent of reaction of Dyestuff synthesis coupling reaction |
| JP2018024787A (en) * | 2016-08-10 | 2018-02-15 | 株式会社サクラクレパス | Colorable ink composition |
Non-Patent Citations (2)
| Title |
|---|
| JUN WANG ET AL: "《201O 2nd Conference on Environmental Science and Information Application Technology》", 31 December 2010 * |
| 王松营: "多聚季铵盐表面活性剂的合成与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112285044A (en) * | 2020-10-27 | 2021-01-29 | 北京大学 | Online differential ultraviolet-visible spectrum detector for organic matters in water and organic matter detection method |
| CN112285044B (en) * | 2020-10-27 | 2022-03-08 | 北京大学 | Online differential ultraviolet-visible spectrum detector for organic matters in water and organic matter detection method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109374608B (en) | 2021-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhu et al. | A colorimetric method for fluoride determination in aqueous samples based on the hydroxyl deprotection reaction of a cyanine dye | |
| US20120329165A1 (en) | Bromate ion measurement method | |
| CN111812047A (en) | Method for determining content of total flavonoids in tobacco based on continuous flow analyzer | |
| CN109374608A (en) | A kind of method of spectrophotometry amine collector | |
| Ahmad | Facial visible spectrophotometric determination of metformin hydrochloride in glucosam tablets and industrial waste water: Application to content uniformity testing | |
| CN102507554A (en) | Method for detecting beryllium content in water | |
| CN113376296B (en) | Method for measuring free formaldehyde content in curing agent | |
| US20130017619A1 (en) | Anionic surfactant detection | |
| CN105223143B (en) | A kind of method of pressure break liquid hold-up in measure oilfield sewage | |
| CN110927091A (en) | Method for quantitatively detecting piperazine water solution | |
| CN111175290A (en) | Water ammonia nitrogen detection reagent and preparation method thereof | |
| CN105277542B (en) | A kind of water nitrite field fast detection method for eliminating reagent blank influence | |
| CN114184607A (en) | System, method and application for determining content of octadecylamine based on ninhydrin | |
| Kara et al. | The sensitive and selective determination of aluminium by spectrofluorimetric detection after complexation with N-o-vanillidine-2-amino-p-cresol | |
| Basavaiah et al. | Spectrophotometric determination of antipsychotic drug olanzapine in pharmaceuticals | |
| CN106872631B (en) | The method for measuring organic impurities in 2- chloromethyl -3- methyl -4- (3- methoxypropoxies) pyridine hydrochloride | |
| CN114910471A (en) | System for determining octadecylamine in potassium chloride and application thereof | |
| Tkáčová et al. | Determination of chlorine dioxide and chlorite in water supply systems by verified methods | |
| CN110146612A (en) | A kind of method of cyanide ion concentration in measurement solution | |
| CN109932360A (en) | A method of quickly measurement Liquor-making industry waste water-residual water total phosphorus | |
| CN114910470A (en) | Method for determining octadecylamine in potassium fertilizer flotation slurry | |
| WO2024007482A1 (en) | Solid reagent for detection of ammonia nitrogen and detection method therefor | |
| CN108344703A (en) | The method of amino benzenes compounds in spectrophotometry water quality | |
| EL SHEIKH et al. | SPECTROPHOTOMETRIC DETERMINATION OF OXYBUTININE HYDROCHLORIDE BY ION-PAIR EXTRACTIONIN IN PHARMACEUTICAL PREPARATIONS | |
| Bagirova et al. | Determination of Tartrazine in Drugs. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | 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 |