CN103063757B - Method for detecting anion-nonionic ampholytic surfactant content in hypersalinity aqueous solution - Google Patents
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Abstract
The invention discloses a method for detecting anion-nonionic ampholytic surfactant content in a hypersalinity aqueous solution. The detection method comprises the following steps of: a: preparing a series of standard solutions; b: constructing a standard curve; c: preparing a sample to be detected; and d: carrying out high performance liquid chromatography detection on the sample to be detected, and calculating the concentration of anion-nonionic ampholytic surfactant in the sample to be detected according to the standard curve by an external standard method. By the method, the anion-nonionic ampholytic surfactant and other substances in a water body can be effectively separated in a chromatographic column, and the content of anion-nonionic ampholytic surfactant content in the hypersalinity aqueous solution is effectively detected. According to the method, only water sample needs to be diluted and filtered, so that the operation is simple and convenient, the processing difficulty is low, and the cost is low.
Description
Technical field
The present invention relates to chemical analysis field, be specifically related to the detection method of concentrated water anions-nonionic amphoteric surfactant content.
Background technology
Anionic-nonionic amphoteric surfactant is the derivant of non-ionics, is further ionized into reactant salt and obtains on the oxyethylene group of non-ionic surfactant, and its molecular structure is mainly: RO (CH
2cH
2o)
ndM, in formula: RO-is hydrophobic grouping, in the majority with alkylol, alkyl phenol, can be also alkyl carboxylic acid, alkylamide etc.;-(CH
2cH
2o)
n-be polyoxyethylene chain, belong to non-ionic hydrophilic group, n is polymerization adduct number;-DM is negative ion alkali, belongs to anionic hydrophilic radical, be mainly-SO of-D
3 -,-PO
3 2-deng acid ion, M is mainly Na
+, K
+deng metallic ion or ethanolamines.In molecular structure due to Anionic-nonionic amphoteric surfactant, there is polyoxyethylene chain and negative ion alkali two parts hydrophilic radical, the ratio that the structure of hydrophilic radical is formed in whole molecule obviously becomes large, thereby make it both there are many functions of non-ionics, there are again a lot of functions of anionic surfactant, present a lot of compatibilities, concertedness physical chemical characteristics, such as hydrophilic ability significantly improves, surfactivity efficiency strengthens, be easy to the features such as long-term storage.
In field of petroleum exploitation, alkyl, polyether sulfonate surfactant is the oil displacement agent using for high temperature and high salt oil deposit, and this class surfactant can effectively improve the oil recovery of high temperature and high salt oil deposit.Because scarcity, the developed field recovery ratio of CNPC's resource are not high, chemical oil displacement agent has become one of important method improving maturing field recovery ratio, surfactant widespread use in tertiary oil recovery.What use was maximum at present is nonionic and anionic surface active agent, as polyoxyethylene octyl phenol ether (OP type) and mahogany sulfonate (PS), but this two classes surfactant all can not be applicable to separately temperature and the high condition of water salinity, single surfactant is not suitable for being applied in high temperature and high salt oil deposit, a little less than anionic surfactant saline-alkaline tolerance, non-ionic surfactant heat resistance is poor, under high temperature and high salt condition, there is strong salt effect, the adsorption precipitation that multivalent ion causes, the defects such as chromatographic resolution, cause existing oil displacement agent not form ultralow interfacial tension with crude oil, do not have due oil displacement efficiency.Therefore, propose nonionic and anionic surface activity functional group to be connected to the Anionic-nonionic amphoteric surfactant in same a part.Anionic-nonionic amphoteric surfactant combines the many merits of anionic and non-ionics, there is good performance, as good in good water-soluble, resisting high temperature, high salt, compatibility, easily biological-degradable and efficiently foaming capacity etc., be particluarly suitable for using under high temperature, high salinity condition.
The present invention relates to lauryl alcohol six sodium sulfonate of ethoxylateds is a kind of Anionic-nonionic amphoteric surfactantes for the designed exploitation of injected water of high salinity, along with the rising of water body salinity, its ability that reduces oil water interfacial tension is higher, and its structural property is subject to the impact of salinity comparatively remarkable.Classical Anionic-nonionic amphoteric surfactant method for separating and analyzing has ion-exchange chromatography and potentiometric titration.Ion-exchange chromatography needs the time of special analytical column and analysis longer, thereby popularity rate is lower; It is larger that potentiometric titration is affected by ionic strength of solution, is not suitable for measuring surfactant concentration in high salinity aqueous solution.If all need Anionic-nonionic amphoteric surfactant to separate or enrichment by ion-exchange chromatography and potentiometric titration, operating process is loaded down with trivial details.And such Anionic-nonionic amphoteric surfactant content of rp-hplc determination that the present invention proposes is relative the most suitable method.
Summary of the invention
In order to solve above-mentioned the problems of the prior art, the invention provides the detection method of concentrated water anions-nonionic amphoteric surfactant content, simple to operation, intractability is low, cost is low.
In order to solve the problems of the technologies described above, the technical scheme that the present invention takes is:
The detection method of concentrated water anions-nonionic amphoteric surfactant content, it comprises the steps:
A. prepare series standard solution: the Anionic-nonionic amphoteric surfactant finished industrial product of getting concentration known, add concentrated water solution preparation to become series standard solution, the salinity of high salinity aqueous solution is less than or equal to 56000mg/L, and high salinity aqueous solution itself is not containing Anionic-nonionic amphoteric surfactant;
B. Criterion curve: series standard solution is carried out to high performance liquid chromatography detection, set up the typical curve of concentrated water anions-nonionic amphoteric surfactant content and peak area;
C. prepare testing sample: get the high salinity aqueous solution distilled water diluting that contains Anionic-nonionic amphoteric surfactant, and filter after as testing sample, described testing sample water is identical with the substrate of standard solution;
D. testing sample is carried out to high performance liquid chromatography detection, calculate the content of Anionic-nonionic amphoteric surfactant in testing sample by external standard method according to typical curve.
Press such scheme, described Anionic-nonionic amphoteric surfactant is one or more in alkyl phenol sulfonic base polyethenoxy ether carboxylate, and general molecular formula is
, wherein R is C
1-C
22alkyl; M is alkaline metal or ammonium; N is any one integer in 1-22.
Press such scheme, described high performance liquid chromatography testing conditions is: chromatographic column is C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water, and flow velocity is 0.5-1ml/min; Column temperature is 30 ℃; Sample size is 5-20 microlitre; Employing UV-detector detects, and wavelength is 224nm.
Press such scheme, described filtration is to adopt 0.45 μ m water system filtering with microporous membrane.
This programme adopts reversed-phased high performace liquid chromatographic to carry out separate targets thing, and reversed phase liquid chromatography adopts the mobile phase (water, methyl alcohol, acetonitrile etc.) of nonpolar fixing phase (wherein C18 bonded silica gel stationary phase uses the most extensive) and polarity.In detachment process, rely on object different with fixing hydrophobic interaction power between mutually and reach the object of separation.And the hydrophobic groups such as aromatic radical, alkyl can produce hydrophobic interaction mutually with fixing, (R is C in the molecule of surfactant of the present invention, to contain hydrophobic phenyl and alkyl
1~ C
22alkyl), these groups are its deciding factors that can be retained, the length of alkyl chain R1 can affect the reservation power of object, if carbochain long (when R1>22), the acting force of itself and fixing phase is excessively strong, can cause the long not even reversible adsorption of disengaging time cannot be by wash-out, therefore R is C here
1~ C
22carbochain; SO
3m(M is alkaline metal or amino) and (CH2CH2O) n is less for the contribution of detachment process, therefore M can be any one in alkaline metal or amino, n can be the arbitrary number in 1 ~ 22.
Compared with prior art, the invention has the advantages that:
1. the content of Anionic-nonionic amphoteric surfactant under existing ion-exchange chromatography and potentiometric determination high salinity, need Surfactant to separate or enrichment, operation easier and cost of determination are improved, detection method of the present invention only need to be diluted and filtration treatment high salinity water sample, simple to operation, intractability is low, cost is low.
2. the present invention has realized Anionic-nonionic amphoteric surfactant and effective separate of other materials in water body in chromatographic column, especially for Anionic-nonionic amphoteric surfactant content analysis in high salinity water body, minimal detectable concentration can reach 20mg/L.
3. the present invention has emphasized that the salinity of solution is on the impact of measurement result, the intensity difference detecting under surfactant solution chromatographic condition under different salinities, the salinity that enters the solution of chromatogram needs strict restriction, and the salinity (being inorganic salts composition and content) of testing sample need to be identical with standard solution.
4. the present invention is applicable to the mensuration of the surface-active contents of Anionic-nonionic amphoteric surfactant in most of high salinity water body, needs only change part chromatographic condition before measuring.
Accompanying drawing explanation
Fig. 1 is the chromatogram of implementing the standard solution that in 1, Anionic-nonionic amphoteric surfactant concentration is 40mg/L.
Fig. 2 is the chromatogram of injection allocation water in embodiment 1.
Fig. 3 ~ 6th, the chromatogram of the titer of different salinities in embodiment 3.
Fig. 7 ~ 10th, the chromatogram of the titer of different salinities in embodiment 4.
Figure 11 is in embodiment 5 when flow rate of mobile phase 1mL/min, the chromatogram of titer.
Embodiment
Below in conjunction with accompanying drawing, embodiment provided by the invention is elaborated.
The instrument that following instance uses: Agilent 1100 high performance liquid chromatographs, variable wavelength scanning UV-detector (VWD), METTLER TOLEDO T70 automatical potentiometric titrimeter; Reagent and source are: Anionic-nonionic amphoteric surfactant finished industrial product is the high-temperature salt-resistant surfactant oil displacement SH03 that Nanjing Chemical Industry Co., Ltd., SINOPEC produces; Acetonitrile is purchased from holder and strangles Migong department, and reagent water is deionized water; Injected water is the injected water of clock city of Hubei Qianjiang City block, and salinity is 280000mg/L; Injection allocation water is clock city of the Hubei Qianjiang City block injected water that is added with the Anionic-nonionic amphoteric surfactant of unknown quantity, and salinity is 280000mg/L.
The Anionic-nonionic amphoteric surfactant finished industrial product of the concentration known described in the present invention, that concrete steps are as follows by the active constituent content of Anionic-nonionic amphoteric surfactant in heterogeneous potentiometric determination Surfactant Industry finished product:
A. storing solution preparation: get finished industrial product standard specimen 0.3000g left and right, add ultrapure water to 100g left and right, prepare the mother liquor of 3000mg/kg, measuring working substance content by potentiometric titration is X left and right, and storing solution concentration is that 3000X mg/kg is for subsequent use;
B. get 2g storing solution, add in the cup of Beckman potentiometric titrimeter, add 20ml deionized water, stir 1min, with the NaOH solution adjusting pH to 11.0 of 0.05mol/L, add again 15ml 4-methyl-2-butanone and 15ml ethanol, stir after 90s, be titrated to terminal with the quick vs of Haier of 0.004mol/L;
C. calculate the effective concentration of Anionic-nonionic amphoteric surfactant in titer, by calculating Anionic-nonionic amphoteric surfactant effective constituent concentration in production piece.
Active principle content
x, numerical value represents with %, calculates by following formula:
x=C × V
e× M × 10
-3/ (W
1× C
0) × 100, in formula:
C---the numerical value of the quick standard titration solution concentration of Haier, unit is mole every liter (mol/L);
V
e---the numerical value of the quick standard titration solution volume of Haier that consumes when equivalent point, unit is milliliter (mL);
The molecular weight of M---sample; The numerical value of the molal weight of sample, unit is gram every mole (g/mol)
W
1---the numerical value of storing solution weight, unit is gram (g);
C
0---the numerical value of surfactant samples compound concentration, unit is grams per kilogram (g/kg).
embodiment 1
The detection method of concentrated water anions-nonionic amphoteric surfactant content, it comprises the steps:
A. prepare series standard solution: the Anionic-nonionic amphoteric surfactant finished industrial product of getting concentration known, add the injected water of clock city of the Hubei Qianjiang City block after diluting 10 times, the storing solution that preparation Anionic-nonionic amphoteric surfactant effective concentration is 1000mg/kg, salinity is 56000mg/L; Get the volumetric flask of 4 50ml, take respectively 1.0g, 2.0g, 4.0g, 10.0g storing solution (being accurate to 0.1mg), clock city of Hubei Qianjiang City block injected water constant volume with dilution after 10 times is to 50ml, the Anionic-nonionic amphoteric surfactant series standard solution that is mixed with 20mg/L, 40mg/L, 80mg/L, 200mg/L, ultrasonic dissolution mixes for subsequent use;
B. Criterion curve: the Anionic-nonionic amphoteric surfactant standard serial solution injecting chromatograph of getting 20mg/L, 40mg/L, 80mg/L, 200mg/L, 1000mg/L carries out analyzing and testing, take sample concentration as horizontal ordinate, peak area is ordinate, the Anionic-nonionic amphoteric surfactant range of linearity is 20-1000mg/L, Criterion curve, regression equation is: Y=1.7944X+6.3127, related coefficient is 0.9992, wherein X represents concentration, and Y represents peak area;
C. prepare testing sample: get No. one, 1ml Jianghan Oil-field clock city station injection allocation water, be settled to 10ml with deionized water, with 0.45 μ m water system membrane filtration, ultrasonic 5min is for subsequent use;
D. testing sample is carried out to high performance liquid chromatography detection, obtains chromatogram as Fig. 2, with Anionic-nonionic amphoteric surfactant effective concentration in external standard method get Gai Zhong city's injection allocation water water sample be 701mg/L.
The chromatogram of the standard solution that Anionic-nonionic amphoteric surfactant concentration is 40mg/L as shown in Figure 1.
The chromatographic condition of note: step b and steps d is: chromatographic column is Zorbax 300SB-C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water; Flow velocity is 0.5ml/min; Column temperature is 30 ℃; Sample size is 20 microlitres; It is 224nm that ultraviolet detects wavelength.
By internal standard method, the middle Anionic-nonionic amphoteric surfactant content analysis result of embodiment 1 testing sample is verified, concrete steps are as follows:
A, get the measured Zhong of 100ml embodiment 1 city's injection allocation water water sample (external standard method measure effective concentration be 701mg/L), be settled to 1000mL with deionized water, obtaining Anionic-nonionic amphoteric surfactant effective concentration is 70.1mg/L, salinity 28000mg/L.
B, get respectively the storing solution (being the storing solution that in embodiment 1, Anionic-nonionic amphoteric surfactant effective concentration is 1000mg/kg) of 2ml, 3ml, 5ml, dilute water sample with the 70.1mg/L of step a and be settled to 50mL, enter respectively chromatograph, each diluted sample do 3 parallel, last calculate recovery rate, measurement result is as shown in table 1.It is accurate to Anionic-nonionic amphoteric surfactant content analysis reliable results in high salinity water body to illustrate according to detection method of the present invention.
The detection method of concentrated water anions-nonionic amphoteric surfactant content, it comprises the steps: a. preparation series standard solution: the Anionic-nonionic amphoteric surfactant finished industrial product of getting concentration known, add the injected water of clock city of the Hubei Qianjiang City block after diluting 5 times, the storing solution that preparation Anionic-nonionic amphoteric surfactant effective concentration is 1000mg/kg, salinity is 56000mg/L; Get the volumetric flask of 4 50ml, take respectively 1.0g, 2.0g, 4.0g, 10.0g storing solution (being accurate to 0.1mg), with diluting 5 Bei Houzhong city block injected water constant volumes to 50ml, the Anionic-nonionic amphoteric surfactant series standard solution that is mixed with 20mg/L, 40mg/L, 80mg/L, 200mg/L, ultrasonic dissolution mixes for subsequent use; B. Criterion curve: the Anionic-nonionic amphoteric surfactant standard serial solution injecting chromatograph of getting 20mg/L, 40mg/L, 80mg/L, 200mg/L, 1000mg/L carries out analyzing and testing, take sample concentration as horizontal ordinate, peak area is ordinate, the Anionic-nonionic amphoteric surfactant range of linearity is 20-1000mg/L, Criterion curve, regression equation is: Y=2.6137X-1.9843, related coefficient is 0.9995, wherein X represents concentration, and Y represents peak area;
C. prepare testing sample: get No. one, 2ml Jianghan Oil-field clock city station injection allocation water, be settled to 10ml with deionized water, with 0.45 μ m water system membrane filtration, ultrasonic 5min is for subsequent use;
D. testing sample is carried out to high performance liquid chromatography detection, with Anionic-nonionic amphoteric surfactant effective concentration in external standard method get Gai Zhong city's injection allocation water water sample be 707mg/L.
The chromatographic condition of note: step b and steps d is: chromatographic column is Zorbax 300SB-C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water; Flow velocity is 0.5ml/min; Column temperature is 30 ℃; Sample size is 20 microlitres; It is 224nm that ultraviolet detects wavelength.
embodiment 3
the present embodiment is that the standard solution of different salinities enters chromatographic contrast test.Step is as follows, and wherein, the chromatographic condition of step b is: chromatographic column is Zorbax 300SB-C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water; Flow velocity is 0.5ml/min; Column temperature is 30 ℃; Sample size is 20 microlitres; It is 224nm that ultraviolet detects wavelength.
A. prepare the standard solution of different salinities: get the Anionic-nonionic amphoteric surfactant finished industrial product of concentration known, be mixed with the standard mother liquor of surfactant effective concentration 3130mg/L with distilled water; Get the volumetric flask of 4 100ml, get the standard mother liquor of 10mL step a, add respectively the injected water of clock city of the Hubei Qianjiang City block of 0mL, 20mL, 50mL, distilled water constant volume, the 4th the volumetric flask injected water constant volume of clock city of Hubei Qianjiang City block, be mixed with the standard solution that salinity is respectively 0mg/L, 56000mg/L, 140000mg/L, 280000mg/L, Anionic-nonionic amphoteric surfactant effective concentration is 313mg/L, with for subsequent use after 0.45 μ m water system membrane filtration;
B. the standard solution of different salinities is carried out to high performance liquid chromatography detection, salinity is respectively the corresponding gained chromatogram of standard solution institute of 0mg/L, 56000mg/L, 140000mg/L, 280000mg/L as Fig. 3 to Fig. 6.
As shown in Figure 3 and Figure 4, salinity is that the peak area that of the standard solution of 0mg/L, 56000mg/L is respectively 315.4 and 795.2, if be respectively 172.3mg/L and 439.6mg/L by the concentration that the typical curve of embodiment 1 calculates, 313.0mg/L does not meet with actual conditions; If calculating the concentration of the standard solution that salinity is 56000mg/L with the typical curve of embodiment 2 is 305.0mg/L, comparatively conform to actual conditions; And Fig. 5 and Fig. 6 be while showing that salinity is more than or equal to 140000mg/L, chromatographic peak serious interference, cannot measure.
Result shows: the present invention relates to Anionic-nonionic amphoteric surfactant solution to be measured, the salinity that enters the solution of chromatogram needs strict restriction, inorganic salts under all measuring conditions composition and content are identical need to be with standard curve making time, therefore according to detection method of the present invention, testing sample salinity should be controlled to 28000mg/L; If the salinity of testing sample, higher than 28000mg/L, should be diluted to 28000mg/L.
Certainly, also can, by improving or reduce the salinity of series standard solution, re-establish typical curve, make the salinity of typical curve identical with testing sample salinity.But while crossing 56000mg/L due to salinity superelevation, chromatographic peak serious interference, cannot measure, therefore when the salinity of standard solution is no more than 56000mg/L, can Criterion curve, thus the content of Anionic-nonionic amphoteric surfactant in testing sample detected.
contrast test when below experiment is 5 microlitre for explanation sample size.Step is as follows, and wherein, the chromatographic condition of step b is: chromatographic column is Zorbax 300SB-C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water; Flow velocity is 0.5ml/min; Column temperature is 30 ℃; Sample size is 5 microlitres; It is 224nm that ultraviolet detects wavelength.
A. get the Anionic-nonionic amphoteric surfactant finished industrial product of concentration known, be mixed with the standard mother liquor of surfactant effective concentration 3130mg/L with distilled water; Get the volumetric flask of 4 100ml, get the standard mother liquor of 10mL step a, add respectively the injected water of clock city of the Hubei Qianjiang City block of 0mL, 20mL, 50mL, distilled water is settled to scale, the 4th volumetric flask is settled to scale with injected water, be mixed with the standard solution that salinity is respectively 0mg/L, 56000mg/L, 140000mg/L, 280000mg/L, Anionic-nonionic amphoteric surfactant effective concentration is 313mg/L, with for subsequent use after 0.45 μ m water system membrane filtration;
B. the standard solution of different salinities is carried out to high performance liquid chromatography detection, salinity is respectively the corresponding gained chromatogram of standard solution institute of 0mg/L, 56000mg/L, 140000mg/L, 280000mg/L as Fig. 7 to Figure 10.
As shown in Figure 7 to 10, salinity is that the peak area that of the standard solution of 0mg/L, 56000mg/L, 140000mg/L, 280000mg/L is respectively 72.4,188.2,158.1 and 133.9, illustrate that by changing sample size be 5 microlitres, chromatographic peak is alleviated with respect to embodiment 2, surfactant in the salinity for higher or high concentration is described, sample size is that 5 microlitres are more suitable for, and can be used for the improvement to the inventive method.
embodiment 5
Below for inquiring into the impact of flow velocity on experimental result.Step is as follows, and wherein, the chromatographic condition of step b is that chromatographic column is Zorbax 300SB-C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water; Flow velocity is 1ml/min; Column temperature is 30 ℃; Sample size is 20 microlitres; It is 224nm that ultraviolet detects wavelength.
A. get the Anionic-nonionic amphoteric surfactant finished industrial product of concentration known, be mixed with the standard mother liquor of surfactant effective concentration 3130mg/L with distilled water, get 10mL in the volumetric flask of a 100ml, and add the injected water 20mL of clock city of Hubei Qianjiang City block, distilled water is settled to scale, obtain the standard solution that salinity is 56000mg/L, Anionic-nonionic amphoteric surfactant effective concentration is 313mg/L, with for subsequent use after 0.45 μ m water system membrane filtration;
B. get step a standard solution injecting chromatograph after treatment, corresponding gained chromatogram is as Figure 11.
According to the peak area of Figure 11, if with the concentration that the typical curve of embodiment 2 calculates the standard solution of the present embodiment be 154mg/L, 313mg/L is not inconsistent with actual concentrations, explanation
Fig. 4 and the present embodiment Figure 11 analyze in 4 in conjunction with the embodiments, and while increasing flow velocity, separating effect is still better, and peak shape is stable, and just retention time reduces, and peak area diminishes to some extent, can be used for method improvement of the present invention.By setting up the typical curve of corresponding flow conditions, also can under this flow conditions, realize testing sample in effective mensuration of Anionic-nonionic amphoteric surfactant content.Therefore, by changing chromatographic condition, set up the typical curve under corresponding chromatographic condition, thereby measure the content of Anionic-nonionic amphoteric surfactant in testing sample, also belong to protection scope of the present invention.
This programme adopts reversed-phased high performace liquid chromatographic to carry out separation and detection object, and reversed phase liquid chromatography adopts the mobile phase (water, methyl alcohol, acetonitrile etc.) of nonpolar fixing phase (wherein C18 bonded silica gel stationary phase uses the most extensive) and polarity.In detachment process, rely on object different with fixing hydrophobic interaction power between mutually and reach the object of separation.In the time there is the hydrophobic group such as alkyl, aromatic radical in object, this hydrophobic interaction power is larger, retain stronger, herein, in the molecule of this surfactant, contain hydrophobic phenyl (one of aromatic radical) and alkyl (alkyl that R1 is C1 ~ C22), therefore as long as Anionic-nonionic amphoteric surfactant is one or more in alkyl phenol sulfonic base polyethenoxy ether carboxylate, just can be suitable for the technical program, be not limited to the Anionic-nonionic amphoteric surfactant adopting in the embodiment of the present invention.
The above is only the preferred embodiment of the present invention, it should be pointed out that the detection of this compounds, is not departing under the prerequisite of the inventive method, can make some improvement and supplement, these improvement and the supplementary protection scope of the present invention that also should be considered as.
Claims (2)
1. the detection method of concentrated water anions-nonionic amphoteric surfactant content, is characterized in that it comprises the steps:
A. prepare series standard solution: get the Anionic-nonionic amphoteric surfactant finished industrial product of concentration known, add concentrated water solution preparation to become series standard solution, the salinity of high salinity aqueous solution is less than or equal to 56000mg/L;
B. Criterion curve: series standard solution is carried out to high performance liquid chromatography detection, set up the content of concentrated water anions-nonionic amphoteric surfactant and the typical curve of peak area;
C. prepare testing sample: get the high salinity aqueous solution distilled water diluting that contains Anionic-nonionic amphoteric surfactant, and filter after as testing sample, described testing sample water is identical with the substrate of standard solution;
D. testing sample is carried out to high performance liquid chromatography detection, with the content of external standard method Anionic-nonionic amphoteric surfactant from typical curve calculating testing sample;
Described high performance liquid chromatography detects and adopts acetonitrile and water as mobile phase;
Described Anionic-nonionic amphoteric surfactant is one or more in alkyl phenol sulfonic base polyethenoxy ether carboxylate, and general molecular formula is
, wherein R is C
1-C
22alkyl; M is alkaline metal or ammonium; N is any one integer in 1-22;
Described high performance liquid chromatography testing conditions is: chromatographic column is C18 post, column length 250mm × internal diameter 4.6mm × particle diameter 5 μ m; Mobile phase is the acetonitrile of volume ratio 4:1 and the mixed liquor of water, and flow velocity is 0.5-1ml/min; Column temperature is 30 ℃; Sample size is 5-20 microlitre; Employing UV-detector detects, and wavelength is 224nm.
2. the detection method of concentrated water anions-nonionic amphoteric surfactant content according to claim 1, is characterized in that described filtration is to adopt 0.45 μ m water system filtering with microporous membrane.
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| 郭霖等.《反相离子对高效液相色谱法分离和测定烷基聚氧乙烯醚羧酸》.《分析化学研究报告》.2000,第28卷(第4期),407-410. |
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