CN102565266B - Ion chromatograph segregation analysis method capable of simultaneously determining four types of alcohol amines in doctor solution - Google Patents
Ion chromatograph segregation analysis method capable of simultaneously determining four types of alcohol amines in doctor solution Download PDFInfo
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- CN102565266B CN102565266B CN201210001630.1A CN201210001630A CN102565266B CN 102565266 B CN102565266 B CN 102565266B CN 201210001630 A CN201210001630 A CN 201210001630A CN 102565266 B CN102565266 B CN 102565266B
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Abstract
The invention relates to an ion chromatograph segregation analysis method for alcohol amines in a doctor solution, in particular to an Ion chromatograph segregation analysis method for four types of alcohol amines in the doctor solution capable of equal-degree separating and suppressing conductivity detection. The method comprises the steps of surveying and mapping a baseline, introducing samples, exchanging ions, eluting, and suppressing conductivity detection analysis. The method can perform good segregation analysis on common alkylol amines in four types of doctor solutions, and relative standard deviations of retention time, peak height and peak area are all less than 2%. Samples are directly injected into an ion chromatograph separation column for separation during analysis, and a spectrogram is acquired through an electric conductivity detector after samples are suppressed by suppressed glue. According the method, a derivative step in the existing method is omitted so that the process is greatly simplified. The method is further used for determining alkylol amine content in a real desulfuration process.
Description
Technical field
The hydramine the present invention relates in doctor solution (comprises isopropanolamine (IPA), triisopropanolamine (TIPA), N methyldiethanol amine (MDEA) and N, N-dimethyl diethanolamine (DMAE)) ion chromatographic separation analytical approach, particularly degree such as grade separates and suppresses electricity and lead the ion chromatographic separation analytical approach of four kinds of hydramine in the doctor solution of detection.
Background technology
In selective desulfurization purified treatment at rock gas, refinery gas, field gas etc. containing H2S and CO2 gas, hydramine method is used widely because having the advantages such as treatment capacity is large, stable operation is reliable.In doctor solution process for preparation, the concentration of desulfurizing agent in doctor solution is had to strict control index, concentration is too high or too low all can cause sulfur content race defective or liquefied gas in liquefied gas to damage.Secondly, removing in sulfuretted hydrogen, carbon dioxide process, in doctor solution can there is degradation Heat of Formation stable salts (heat-stable salts is called for short HSS) in hydramine, and the generation of HSS is the major reason that causes equipment corrosion to aggravate with accumulation.Therefore, thereby in sulfur removal technology, the detection of desulfurizing agent is ensured to desulfurized effect so that its content is strictly controlled, become necessary links.In domestic factory, measuring the conventional method of hydramine concentration in doctor solution is acid base neutralization titration method, the method process is loaded down with trivial details, and analysis time is long, and because acid base titration selectivity is not high, in doctor solution, other alkaline impurities serious interference, bring serious error to detection.Vapor-phase chromatography generally need be through derivative to the mensuration of amine, complex operation, consuming time, and carrier used is expensive, the most important thing is, removing in sulfuretted hydrogen, carbon dioxide process, in doctor solution, the existence of the material such as sulfuretted hydrogen has had a strong impact on the mensuration in gas chromatography.
Summary of the invention
The deficiency that the present invention exists for prior art, method just, provides the ion chromatographic separation analytical approach of four kinds of hydramine in a kind of doctor solution, and the method can ensure analytical effect, again can simplification of flowsheet, do not need derivative can mensuration.
Concrete technical scheme of the present invention is as follows:
The present invention is a kind of ion chromatographic separation analytical approach of simultaneously measuring four kinds of hydramine in doctor solution, comprises the following steps:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, flow into conductance flow cell from the eluent of chromatography column output, be converted into electric signal by electric conductivity detector, surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample enters chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is inputted in chromatography column continuously, constantly hydramine and Common Cations are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppressing electricity leads to detect and analyzes: during by conductance cell through electric conductivity detector be converted into electric signal by suppressing glue after suppressing from the alkanolamine solution of chromatography column output, thereby formation spectrogram is recorded.
Hydramine in doctor solution of the present invention is isopropanolamine (IPA), and eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, and 0.5mM L-Histidine mixed solution, adopts isocratic elution.
Hydramine in doctor solution of the present invention is triisopropanolamine (TIPA), and eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, and 0.5mM L-Histidine mixed solution, adopts isocratic elution.
Hydramine in doctor solution of the present invention is N methyldiethanol amine (MDEA), and eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, and 0.5mM L-Histidine mixed solution, adopts isocratic elution.
Hydramine in doctor solution of the present invention is N, N-dimethyl diethanolamine (DMAE), and eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, 0.5mM L-Histidine mixed solution, adopts isocratic elution.
Separating column of the present invention is TSK gelSuper IC-CR cation exchange column, and sample size is 30 μ L.
The present invention has following beneficial effect:
1. in pair four kinds of doctor solutions, conventional hydramine can carry out good compartment analysis, and the relative standard deviation of retention time, peak height, peak area is all less than 2%, and lowest detectable limit can reach 10
-7g/L, in 0.2mg/L～20mg/L concentration range, peak height is good linear relationship to concentration, peak area to concentration, and related coefficient is more than 0.998;
2. while analysis, sample is directly injected to ion chromatographic separation post and separate, suppress just can obtain spectrogram through electric conductivity detector afterwards by suppressing glue, remove the derivative step in existing method, technological process is greatly simplified;
3. this method can be used for the detection of the alcohol amine content in practical sulphur removal technique.
Brief description of the drawings
Fig. 1 is four kinds of hydramine and six kinds of cationic mixed standard solution chromatograms in the doctor solution obtaining according to method provided by the invention; In figure, 1=Li
+, 2=Na
+, 3=DMAE, 4=MDEA, 5=TIPA, 6=NH4
+, 7=IPA, 8=Mg
2+, 9=Ca
2+, 10=K
+;
Fig. 2 is hydramine chromatogram in the actual sample doctor solution (lean solution) obtaining according to method provided by the invention, in figure, and 1=Na
+, 2=DMAE, 3=MDEA, 4=unkown, 5=NH
4 +, 6=Mg
2+, 7=Ca
2+, 8=K
+.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described in detail:
Processing step comprise successively mapping, sample introduction and ion-exchange, wash-out, non-electricity processed lead detect analyze:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, flow into conductance flow cell from the eluent of chromatography column output, be converted into electric signal by electric conductivity detector, surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample enters chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is inputted in chromatography column continuously, constantly hydramine and Common Cations are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppressing electricity leads to detect and analyzes: during by conductance cell through electric conductivity detector be converted into electric signal by suppressing glue after suppressing from the alkanolamine solution of chromatography column output, thereby formation spectrogram is recorded.
While analyzing above-mentioned alkanolamine solution, separating column is TSK gelSuper IC-CR cation exchange column, and eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, and the mixed solution of 0.5mM L-Histidine, sample size is 30 μ L, adopts isocratic elution.
Describe the present invention in detail below in conjunction with accompanying drawing:
Embodiment:
The present embodiment is that the lean solution sample containing desulfurizing agent in production run is analyzed
Use instrument: TOSOH IC-2010 ion chromatograph (TOSOH), TSK guardcolumn Super IC-C HS (4.6mm*1cm), TSK gelSuper IC-CR (4.6mm*10cm, m), kation suppresses glue (TOSOH) to 3 μ; TSK gelSuper IC-CR cation exchange column, 30 μ L quantitatively encircle; Flow velocity: 1.0mL/min; Column temperature: 40 DEG C; Sample size: 30 μ L;
Detection mode: suppress electricity and lead detection; Data processing: TOSOH IC-2010 chromatographic work station;
Eluent: 2.0mM crown ether, 2.2mM pyrovinic acid, the mixed solution of 0.5mM L-Histidine;
Analytical procedure:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, flow into conductance flow cell from the eluent of chromatography column output, be converted into electric signal by electric conductivity detector, surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample enters chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is inputted in chromatography column continuously, constantly hydramine and Common Cations are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppressing electricity leads to detect and analyzes: from the alkanolamine solution of chromatography column output by suppress glue suppress after during by conductance cell process electric conductivity detector be converted into electric signal, be recorded thereby form spectrogram, the Fig. 1 surveying and drawing is four kinds of hydramine and six kinds of cationic mixed standard solution chromatograms in the doctor solution obtaining according to method provided by the invention; In figure, 1=Li
+, 2=Na
+, 3=DMAE, 4=MDEA, 5=TIPA, 6=NH4
+, 7=IPA, 8=Mg
2+, 9=Ca
2+, 10=K
+; Fig. 2 is hydramine chromatogram in the actual sample doctor solution (lean solution) obtaining according to method provided by the invention, in figure, and 1=Na
+, 2=DMAE, 3=MDEA, 4=unkown, 5=NH
4 +, 6=Mg
2+, 7=Ca
2+, 8=K
+.
Analysis result:
As calculated, in this lean solution, DMAE content is that 6.6%, MDEA content is 34.8%.TIPA and IPA do not detect, in sample, DMAE and MDEA average recovery rate are respectively 103.15%, 95.48%, and the recovery of standard addition of TIPA and IPA is respectively 97.64%, 92.41%.
Above-described embodiment is used for the present invention that explains, instead of limits the invention, and in spirit of the present invention and claim protection domain, any amendment and change that the present invention is made, all fall into protection scope of the present invention.
Claims (1)
1. an ion chromatographic separation analytical approach of simultaneously measuring four kinds of hydramine in doctor solution, is characterized in that, comprises the following steps:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, flow into conductance flow cell from the eluent of chromatography column output, be converted into electric signal by electric conductivity detector, surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample enters chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is inputted in chromatography column continuously, constantly hydramine and Common Cations are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppressing electricity leads to detect and analyzes: during by conductance cell through electric conductivity detector be converted into electric signal by suppressing glue after suppressing from the alkanolamine solution of chromatography column output, thereby formation spectrogram is recorded;
Hydramine in described doctor solution is isopropanolamine (IPA), triisopropanolamine (TIPA), N methyldiethanol amine (MDEA) or N, N-dimethyl diethanolamine (DMAE), described eluent is 2.0mM crown ether, 2.2mM pyrovinic acid, 0.5mML-histidine mixed solution, adopt isocratic elution, described separating column is TSK gelSuper IC-CR cation exchange column, and sample size is 30 μ L.
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| CN103529157A (en) * | 2013-10-08 | 2014-01-22 | 中华人民共和国北京出入境检验检疫局 | Ion chromatography-mass spectrometry detection method of migration volumes of amine curing agents in water purification resins |
| CN106442804B (en) * | 2016-11-23 | 2019-01-15 | 福建出入境检验检疫局检验检疫技术中心 | The detection method of alcamines material transport amount in a kind of Plastics |
| CN106918669B (en) * | 2017-02-21 | 2019-09-03 | 华润水泥技术研发有限公司 | The detection method of alcohols, alcamine compound in grinding aid |
| CN107328877A (en) * | 2017-06-30 | 2017-11-07 | 黄河三角洲京博化工研究院有限公司 | A kind of method of N methyl diethanolamine contents in LC-MS analysis water |
| CN110646531A (en) * | 2019-09-18 | 2020-01-03 | 湘潭大学 | Ion chromatography quantitative analysis method for raw material diethanolamine in reaction liquid for synthesizing iminodiacetic acid by dehydrogenation of diethanolamine |
| CN112782288B (en) * | 2019-11-06 | 2023-05-09 | 中国石油化工股份有限公司 | Separation detection method for amine and impurities in amine-containing aqueous solution |
| CN112781794B (en) * | 2019-11-06 | 2023-09-15 | 中国石油化工股份有限公司 | Online monitoring method and system for leakage of amine liquid water cooler |
| CN111474249A (en) * | 2020-03-11 | 2020-07-31 | 台州学院 | Method for detecting organic alcohol amine compounds in environmental water sample |
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Non-Patent Citations (4)
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| N-甲基二乙醇胺脱硫液中热稳态盐的分析;汪文强等;《石油化工》;20071231;第36卷(第1期);第89-91页第2-3节 * |
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| 汪文强等.N-甲基二乙醇胺脱硫液中热稳态盐的分析.《石油化工》.2007,第36卷(第1期),第88-91页. * |
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