CN105115957A - Quantitative detection method for hexadecyl trimethyl ammonium bromide - Google Patents
Quantitative detection method for hexadecyl trimethyl ammonium bromide Download PDFInfo
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- CN105115957A CN105115957A CN201510442613.5A CN201510442613A CN105115957A CN 105115957 A CN105115957 A CN 105115957A CN 201510442613 A CN201510442613 A CN 201510442613A CN 105115957 A CN105115957 A CN 105115957A
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- trimethyl ammonium
- ctab
- ammonium bromide
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Abstract
The invention provides a quantitative detection method for hexadecyl trimethyl ammonium bromide, and relates to a method for detecting hexadecyl trimethyl ammonium bromide. The detection method solves the technical problems that the detection limit is high and operation is tedious in present hexadecyl trimethyl ammonium bromide detection methods. The method comprises steps: silver nitrate is dissolved in water, a sodium citrate solution is added in a heating condition for reduction, and silver sol is obtained; a hexadecyl trimethyl ammonium bromide solution is added into the silver soil, the mixture is mixed uniformly, and a series of CTAB-AgNPs mixed liquids with different concentrations are obtained, Raman spectrum test is carried out, a picture of intensities of characteristic peaks in the Raman spectra to CTAB concentrations is drawn, a standard curve is obtained, then a liquid to be detected is mixed with the silver sol, Raman spectrum test is carried out, the concentration of hexadecyl trimethyl ammonium bromide in the substance to be detected is obtained from the standard curve. The detection limit can reach a minimum of 7.4*10<-7>M. The detection method can be used for detection of CTAB in surface water, lake water and sewage.
Description
Technical field
The present invention relates to the method detecting cetyl trimethyl ammonium bromide (CTAB).
Background technology
Along with the development of modern industry, the consumption of surfactant sharply increases, and brings more and more serious pollution and harm to ecologic environment.Wherein, cationic surfactant, as the larger organic contaminant of a class toxicity, has strong inhibiting effect to microorganism, in the environment not easily biological-degradable, also suppresses the degraded of other pollutant simultaneously, can cause serious water pollution.Cetyl trimethyl ammonium bromide (CTAB) is important cationic surfactant, there are the performances such as excellent infiltration, softening, emulsification, antistatic and sterilization, be widely used in, in commercial production and daily product, being released to the most at last in environment, causing environmental problem.Therefore, set up detection and the quantivative approach of CTAB, have Special Significance for biological, chemistry, environment and medical science etc.Qian etc. disclose one section of article " a kind of supramolecular system on-off role in fluorescent molecule switch for detecting cationic surfactant and logic gate " (ASupramolecularOff-OnFluorescentSwitchandIMPLICATIONLogi cGateforDetectionofCationicSurfactant) at the 1015-1020 page of " fluorescence magazine " (JournalofFluorescence) the 21st volume the 3rd phase in 2011, adopt a kind of supramolecular system to utilize the principle of fluorescence indicator competitive displacement to detect CTAB in literary composition, detection limit is 3 × 10
-6m; Su Fengyi, Xing Xinhui be article " utilizing fluorescein isothiocyanate to detect the method for quaternary cationics " disclosed in the 2589-2595 page of " Journal of Chemical Industry and Engineering " the 59th volume the 10th phase in 2008, use in literary composition fluorescein isothiocyanate (FITC) to quaternary cationics in aqueous concentration carried out quantitative detection, be 1.7 × 10 to the detection limit of CTAB
-6m, quantification range is 1.7 × 10
-6m ~ 0.27 × 10
-3m.All there is the shortcoming detecting limit for height, complex operation in above method.
Summary of the invention
The present invention solves the technical matters that existing cetyl trimethyl ammonium bromide (CTAB) detection method detects limit for height, complex operation, and provides a kind of quantitative detecting method of cetyl trimethyl ammonium bromide.
The quantitative detecting method of cetyl trimethyl ammonium bromide of the present invention, carries out according to the following steps:
One, taking 18.0mg ~ 72.0mg silver nitrate is dissolved in 150mL water, under agitation, after being heated to boiling, add the sodium citrate solution that 2.0mL ~ 8.0mL mass percentage concentration is 1% ~ 3% again, continue to keep solution seethe with excitement and stir 30 ~ 60min, naturally cool to room temperature, obtain silver sol, silver sol is kept in Dark Place for subsequent use at 0 ~ 4 DEG C;
Two, isopyknic silver sol 4 ~ 10 parts prepared by step one is got, add the cetyl trimethyl ammonium bromide solution of different volumes wherein, be mixed with the CTAB-AgNPs mixed liquor of a series of different CTAB concentration, after leaving standstill 3 ~ 5min, carry out Raman spectrum test, with 759cm in Raman spectrum
-1, 1230cm
-1or 1442cm
-1characteristic peak intensity to CTAB concentration mapping, obtain typical curve;
Three, the silver sol 1 part with step 2 same volume is got, add the test substance containing cetyl trimethyl ammonium bromide wherein, obtain CTAB-AgNPs mixed liquor to be measured, carry out the test of Raman spectrum, obtain the intensity level of the characteristic peak identical with step 2, on typical curve, find the concentration of cetyl trimethyl ammonium bromide in test substance with this intensity level, complete the quantitative detection of cetyl trimethyl ammonium bromide.
The present invention first uses reduction of sodium citrate legal system for the nano silver colloidal sol AgNPs of even particle size distribution, and the active substrate tested using nano silver colloidal sol as Raman spectrum detects CTAB.In aqueous, CTAB, by the electrostatic interaction between nano silver colloidal sol, carries out self assembly on silver nano-grain surface, causes silver nano-grain to assemble.Formed and there is the active substrate that better Raman strengthens effect, thus realize the detection to CTAB.This active substrate, can from Common Cations surfactant, anionic surfactant and non-ionic surfactant selective enumeration method CTAB.Method of the present invention is without the need to adding any probe molecule, quick, sensitive, selectivity is high, and repeatability is good, and detection limit is minimum reaches 7.4 × 10
-7m.Achieve the real-time, quick, sensitive of CTAB and selective enumeration method.Can be applicable to actual environment water sample, the detection of such as, quaternary cationics CTAB in surface water, lake water and sewage etc.
Accompanying drawing explanation
Fig. 1 is Common surface activating agent and the mixed Raman spectrogram of silver sol of embodiment 1.
Fig. 2 is that the CTAB concentration of embodiment 1 is respectively 1.0 × 10
-6, 1.5 × 10
-6, 2.0 × 10
-6, 2.5 × 10
-6, 3.5 × 10
-6, 5.0 × 10
-6, 7.5 × 10
-6the silver sol of M and the Raman spectrogram of CTAB mixed system.
Fig. 3 is the Raman characteristic peak 759cm of the CTAB of embodiment 1
-1intensity and the linear relationship chart of CTAB concentration.
Fig. 4 is the Raman characteristic peak 759cm of the CTAB of embodiment 2
-1intensity and the linear relationship chart of CTAB concentration.
Embodiment
Embodiment one: the quantitative detecting method of the cetyl trimethyl ammonium bromide of present embodiment, carry out according to the following steps:
One, taking 18.0mg ~ 72.0mg silver nitrate is dissolved in 150mL water, under agitation, after being heated to boiling, add the sodium citrate solution that 2.0mL ~ 8.0mL mass percentage concentration is 1% ~ 3% again, continue to keep solution seethe with excitement and stir 30 ~ 60min, naturally cool to room temperature, obtain silver sol, silver sol is kept in Dark Place for subsequent use at 0 ~ 4 DEG C;
Two, isopyknic silver sol 4 ~ 10 parts prepared by step one is got, add the cetyl trimethyl ammonium bromide solution of different volumes wherein, be mixed with the CTAB-AgNPs mixed liquor of a series of different CTAB concentration, after leaving standstill 3 ~ 5min, carry out Raman spectrum test, with 759cm in Raman spectrum
-1, 1230cm
-1or 1442cm
-1characteristic peak intensity to CTAB concentration mapping, obtain typical curve;
Three, the silver sol 1 part with step 2 same volume is got, add the test substance containing cetyl trimethyl ammonium bromide wherein, obtain CTAB-AgNPs mixed liquor to be measured, carry out the test of Raman spectrum, obtain the intensity level of the characteristic peak identical with step 2, on typical curve, find the concentration of cetyl trimethyl ammonium bromide in test substance with this intensity level, complete the quantitative detection of cetyl trimethyl ammonium bromide.
Embodiment two: present embodiment and embodiment one are 100 ~ 500 revs/min unlike the rotating speed stirred in step one.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are dissolved in 150mL water unlike taking 30.0mg silver nitrate in step one, under agitation, after being heated to boiling, add the sodium citrate solution that 3.0mL mass percentage concentration is 2% again, continue to keep solution seethe with excitement and stir 40min, naturally cool to room temperature, obtain silver sol.Other are identical with embodiment one.
Embodiment four: present embodiment and embodiment one are dissolved in 150mL water unlike taking 40.0mg silver nitrate in step one, under agitation, after being heated to boiling, add the sodium citrate solution that 5.0mL mass percentage concentration is 3% again, continue to keep solution seethe with excitement and stir 20min, naturally cool to room temperature, obtain silver sol.Other are identical with embodiment one.
Embodiment five: one of present embodiment and embodiment one to four are 8.0 × 10 unlike CTAB concentration in CTAB-AgNPs system in step 2
-7m ~ 1.0 × 10
-5m.Other are identical with one of embodiment one to four.
Be further described the inventive method below in conjunction with specific embodiment, to understand the present invention with it will be apparent to those skilled in that, but following examples do not limit the scope of request of the present invention protection in any form.
Embodiment one
Test 1: the selectivity demonstration test of the quantitative detecting method of cetyl trimethyl ammonium bromide, carry out according to the following steps:
One, taking 36.0mg silver nitrate is dissolved in 150mL water, under speed of agitator is 500 revs/min of conditions, after being heated to boiling, add the sodium citrate solution that 4.0mL mass percentage concentration is 1% again, continue to keep solution seethe with excitement and stir 30min, naturally cool to room temperature, obtain bluish yellow look silver sol, silver sol is kept in Dark Place for subsequent use at 4 DEG C;
Two, by surfactant cetyl trimethyl ammonium bromide (CTAB), dodecyl benzyl dimethyl ammonium chloride (DDBAC), cetylpyridinium chloride (CPC), DTAB (DTAB), P123 (PEO-PPO-PEO), lauric monoglyceride (GML), dialkyl benzene sulfonic acids sodium (SDBS), polyoxyethylene ether (AEO
3), sodium dodecylsulphonate (DOSO
3na), lauryl sodium sulfate (DSO
4na) and NPE (OP-10) mix with 2.0mL silver sol respectively, surfactant concentration is all 1.0 × 10
-5m, after leaving standstill 3min, carries out Raman spectrum test.The Raman spectrogram obtained as shown in Figure 1, is followed successively by 1 to 11 in Fig. 1 from top to bottom, and wherein 1 is CTAB, and 2 is DDBAC, and 3 is CPC, and 4 is DTAB, and 5 is PEO-PPO-PEO, and 6 is GML, and 7 is SDBS, and 8 is AEO, and 9 is DOSO
3na, 10 is DSO
4na, 11 is OP-10.The Raman signal of non-ionic surfactant and anionic surfactant is not all well strengthened as can be seen from Figure 1, the Raman signal intensity of cationic surfactant then all improves, but its Raman spectrum is obviously different from the Raman spectrum of CTAB, and their Raman spectrum is at the characteristic peak 759cm of CTAB
-1all there is not stronger Raman peaks in place.Thus show, this method can selective enumeration method cetyl trimethyl ammonium bromide (CTAB).In figure: ordinate represents the intensity of raman characteristic peak, and horizontal ordinate represents Raman shift.
Test 2: the quantitative detecting method of cetyl trimethyl ammonium bromide in the actual environment water sample of this test, carry out according to the following steps:
One, taking 36.0mg silver nitrate is dissolved in 150mL water, under speed of agitator is 400 revs/min of conditions, after being heated to boiling, add the sodium citrate solution that 4.0mL mass percentage concentration is 2% again, continue to keep solution seethe with excitement and stir 30min, naturally cool to room temperature, obtain bluish yellow look silver sol, silver sol is kept in Dark Place for subsequent use at 4 DEG C;
Two, get the silver sol 7 parts of 2.0mL prepared by step one, the concentration adding different volumes is wherein 1.0 × 10
-3the cetyl trimethyl ammonium bromide solution of mol/L, be mixed with the CTAB-AgNPs mixed liquor of a series of different CTAB concentration, in mixed liquor, CTAB concentration is respectively 1.0 × 10
-6mol/L, 1.5 × 10
-6mol/L, 2.0 × 10
-6mol/L, 2.5 × 10
-6mol/L, 3.5 × 10
-6mol/L, 5.0 × 10
-6mol/L, 7.5 × 10
-6mol/L, leaves standstill after 3min, carries out Raman spectrum test, the Raman spectrogram obtained as shown in Figure 2,759cm in Raman spectrum in Fig. 2
-1characteristic peak intensity to CTAB concentration mapping as shown in Figure 3, obtain typical curve;
As can be seen from Figure 3, along with the increase of CTAB concentration, characteristic peak 759cm
-1intensity strengthen gradually.As can be seen from Figure 3, when CTAB concentration is 1.0 × 10
-6m ~ 7.5 × 10
-6within the scope of M, the characteristic peak 759cm of CTAB
-1peak area and the concentration of CTAB present good linear relationship (R
2=0.9894).Carry out 20 average measurement to blank sample, by 3 σ/K (σ is zero standard deviation, and K is regression equation slope), calculating detects and is limited to 7.9 × 10
-7m.Show, the detection sensitivity of this method to CTAB is high, and detection limit is low.
Three, not to be subject to surface water and the lake water of CTAB pollution, surface water and lake water qualitative filter paper are filtered, is then separated with 12000rpm with centrifugal separator.In the lake water after this process, add CTAB, obtain CTAB aqueous solution.Get the silver sol of 2.0mL step one preparation, and add CTAB aqueous solution in silver sol, obtain CTAB concentration and be respectively 1.0 × 10
-6m, 3.0 × 10
-6m and 6.0 × 10
-6the CTAB of M and the mixed solution of silver sol, leave standstill 3min, carry out the test of Raman spectrum.Obtain 759cm
-1characteristic peak intensity, on typical curve, find the concentration of cetyl trimethyl ammonium bromide in water sample to be measured with this intensity level.By contrasting with quantitation curves, obtaining the actual detectable concentration of CTAB, calculating the recovery, be listed in the table below in 1,
The detected value of the CTAB in table 1 actual environment water sample
Show from the result of table 1, the recovery, between 98.9 ~ 100.2%, obtains good experimental result, proves that this method can be applicable to the detection of the CTAB in actual environment water sample.
Embodiment 2
Test 1: the selectivity demonstration test of the quantitative detecting method of cetyl trimethyl ammonium bromide, carry out according to the following steps:
One, taking 27.0mg silver nitrate is dissolved in 150mL water, under speed of agitator is 300 revs/min of conditions, after being heated to boiling, add the sodium citrate solution that 3.0mL mass percentage concentration is 3% again, continue to keep solution seethe with excitement and stir 30min, naturally cool to room temperature, obtain bluish yellow look silver sol, silver sol is kept in Dark Place for subsequent use at 4 DEG C;
Two, by surfactant cetyl trimethyl ammonium bromide (CTAB), dodecyl benzyl dimethyl ammonium chloride (DDBAC), cetylpyridinium chloride (CPC), DTAB (DTAB), P123 (PEO-PPO-PEO), lauric monoglyceride (GML), dialkyl benzene sulfonic acids sodium (SDBS), polyoxyethylene ether (AEO
3), sodium dodecylsulphonate (DOSO
3na), lauryl sodium sulfate (DSO
4na) and NPE (OP-10) mix with 2.0mL silver sol respectively, surfactant concentration is all 1.0 × 10
-5m, after leaving standstill 3min, carries out Raman spectrum test.Raman spectrum shows that the Raman signal of non-ionic surfactant and anionic surfactant is not all well strengthened, the Raman signal intensity of cationic surfactant then all improves, but its Raman spectrum is obviously different from the Raman spectrum of CTAB, and their Raman spectrum is at the characteristic peak 759cm of CTAB
-1all there is not stronger Raman peaks in place.Therefore this method can selective enumeration method cetyl trimethyl ammonium bromide (CTAB).
Test 2: the quantitative detecting method of cetyl trimethyl ammonium bromide in the actual environment water sample of this test, carry out according to the following steps:
One, taking 27.0mg silver nitrate is dissolved in 150mL water, under speed of agitator is 100 ~ 500 revs/min of conditions, after being heated to boiling, add the sodium citrate solution that 3.0mL mass percentage concentration is 3% again, continue to keep solution seethe with excitement and stir 30min, naturally cool to room temperature, obtain bluish yellow look silver sol, silver sol is kept in Dark Place for subsequent use at 4 DEG C;
Two, get the silver sol 7 parts of 2.0mL prepared by step one, the concentration adding different volumes is wherein 1.0 × 10
-3the cetyl trimethyl ammonium bromide solution of mol/L, be mixed with the CTAB-AgNPs mixed liquor of a series of different CTAB concentration, in mixed liquor, CTAB concentration is respectively 1.0 × 10
-6mol/L, 1.5 × 10
-6mol/L, 2.0 × 10
-6mol/L, 2.5 × 10
-6mol/L, 3.5 × 10
-6mol/L, 5.0 × 10
-6mol/L, 7.5 × 10
-6mol/L, after leaving standstill 3min, carries out Raman spectrum test, with 759cm in Raman spectrum
-1characteristic peak intensity to CTAB concentration mapping, obtain typical curve, as shown in Figure 4.
As can be seen from Figure 4, along with the increase of CTAB concentration, characteristic peak 759cm
-1intensity strengthen gradually.When CTAB concentration is 1.0 × 10
-6m ~ 7.5 × 10
-6within the scope of M, the characteristic peak 759cm of CTAB
-1peak area and the concentration of CTAB present good linear relationship (R
2=0.9897).Carry out 20 average measurement to blank sample, by 3 σ/K (σ is zero standard deviation, and K is regression equation slope), calculating detects and is limited to 7.4 × 10
-7m.Show, the detection sensitivity of this method to CTAB is high, and detection limit is low.
Three, for the surface water polluted by CTAB and lake water, surface water and lake water qualitative filter paper are filtered, is then separated with 12000rpm with centrifugal separator.In the lake water after this process, add CTAB, obtain CTAB aqueous solution.Get the silver sol of 2.0mL step one preparation, and add CTAB aqueous solution in silver sol, obtain CTAB concentration and be respectively 1.0 × 10
-6m, 3.0 × 10
-6m and 6.0 × 10
-6the CTAB of M and the mixed solution of silver sol, leave standstill 3min, carry out the test of Raman spectrum.Obtain 759cm
-1characteristic peak intensity, on typical curve, find the concentration of cetyl trimethyl ammonium bromide in water sample to be measured with this intensity level.By contrasting with quantitation curves, obtaining the actual detectable concentration of CTAB, calculating the recovery, be listed in the table below in 2,
The detected value of the CTAB in table 2 actual environment water sample
Show from the result of table 2, the recovery between 99.7 ~ 100.3% between, obtain good experimental result, prove that this method can be applicable to the detection of the CTAB in actual environment water sample.
Claims (5)
1. a quantitative detecting method for cetyl trimethyl ammonium bromide, is characterized in that the method is carried out according to the following steps:
One, taking 18.0mg ~ 72.0mg silver nitrate is dissolved in 150mL water, under agitation, after being heated to boiling, add the sodium citrate solution that 2.0mL ~ 8.0mL mass percentage concentration is 1% ~ 3% again, continue to keep solution seethe with excitement and stir 30 ~ 60min, naturally cool to room temperature, obtain silver sol, silver sol is kept in Dark Place for subsequent use at 0 ~ 4 DEG C;
Two, isopyknic silver sol 4 ~ 10 parts prepared by step one is got, add the cetyl trimethyl ammonium bromide solution of different volumes wherein, be mixed with the CTAB-AgNPs mixed liquor of a series of different CTAB concentration, after leaving standstill 3 ~ 5min, carry out Raman spectrum test, with 759cm in Raman spectrum
-1, 1230cm
-1or 1442cm
-1characteristic peak intensity to CTAB concentration mapping, obtain typical curve;
Three, the silver sol 1 part with step 2 same volume is got, add the test substance containing cetyl trimethyl ammonium bromide wherein, obtain CTAB-AgNPs mixed liquor to be measured, carry out the test of Raman spectrum, obtain the intensity level of the characteristic peak identical with step 2, on typical curve, find the concentration of cetyl trimethyl ammonium bromide in test substance with this intensity level, complete the quantitative detection of cetyl trimethyl ammonium bromide.
2. the quantitative detecting method of a kind of cetyl trimethyl ammonium bromide according to claim 1, is characterized in that the rotating speed stirred in step one is 100 ~ 500 revs/min.
3. the quantitative detecting method of a kind of cetyl trimethyl ammonium bromide according to claim 1 and 2, it is characterized in that taking 30.0mg silver nitrate in step one is dissolved in 150mL water, under agitation, after being heated to boiling, add the sodium citrate solution that 3.0mL mass percentage concentration is 2% again, continue to keep solution seethe with excitement and stir 40min, naturally cool to room temperature, obtain silver sol.
4. the quantitative detecting method of a kind of cetyl trimethyl ammonium bromide according to claim 1 and 2, it is characterized in that taking 40.0mg silver nitrate in step one is dissolved in 150mL water, under agitation, after being heated to boiling, add the sodium citrate solution that 5.0mL mass percentage concentration is 3% again, continue to keep solution seethe with excitement and stir 20min, naturally cool to room temperature, obtain silver sol.
5. the quantitative detecting method of a kind of cetyl trimethyl ammonium bromide according to claim 1 and 2, is characterized in that in step 2, in CTAB-AgNPs system, CTAB concentration is 8.0 × 10
-7~ 1.0 × 10
-5mol/L.
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Cited By (1)
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| CN107884384A (en) * | 2017-11-13 | 2018-04-06 | 山东深海海洋科技有限公司 | Nitrate nitrogen Raman detection analysis method based on nitrate enhancing Nano Silver |
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