CN102565266A - 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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- CN102565266A CN102565266A CN2012100016301A CN201210001630A CN102565266A CN 102565266 A CN102565266 A CN 102565266A CN 2012100016301 A CN2012100016301 A CN 2012100016301A CN 201210001630 A CN201210001630 A CN 201210001630A CN 102565266 A CN102565266 A CN 102565266A
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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 that the present invention relates in the doctor solution (comprises isopropanolamine (IPA); Triisopropanolamine (TIPA); N methyldiethanol amine (MDEA) and N; N-dimethyl diethanolamine (DMAE)) ion chromatographic separation analytical approach, particularly degree of grade separates and suppresses the ion chromatographic separation analytical approach that electricity is led four kinds of hydramine in the doctor solution of detection.
Background technology
Contain in the selective desulfurization purified treatment of H2S and CO2 gas at rock gas, refinery gas, field gas etc., the hydramine method is used widely because of having advantages such as treatment capacity is big, stable operation is reliable.In the doctor solution process for preparation, the concentration of desulfurizing agent in the doctor solution there is strict controlling index, concentration is too high or too low all can to cause in the liquefied gas sulfur content race defective or liquefied gas to decrease.Secondly, in removing sulfuretted hydrogen, carbon dioxide process, degradation generation thermal-stable salt (heat-stable salts is called for short HSS) can take place in hydramine in the doctor solution, and the generation of HSS is the major reason that causes the equipment corrosion aggravation with accumulation.Therefore, thereby in sulfur removal technology, the detection of desulfurizing agent is guaranteed desulfurized effect its content is carried out strictness control, become necessary link.Measuring the method that hydramine concentration is used always in the doctor solution in the domestic factory is the acid base neutralization titration method; The method process is loaded down with trivial details, and analysis time is long, and because the acid base titration selectivity is not high; Other alkaline impurities serious interference are brought serious error to detection in the doctor solution.Vapor-phase chromatography generally need be passed through the mensuration of amine and derived; Complex operation, consuming time, and used carrier costs an arm and a leg, and the most important thing is; In removing sulfuretted hydrogen, carbon dioxide process, the existence of material such as sulfuretted hydrogen has had a strong impact on the mensuration in the gas chromatography in the doctor solution.
Summary of the invention
The present invention provides the ion chromatographic separation analytical approach of four kinds of hydramine in a kind of doctor solution just to the deficiency of prior art, method existence, and the method can guarantee analytical effect, can simplify technological process again, need not derive and can measure.
Concrete technical scheme of the present invention is following:
The present invention is a kind of ion chromatographic separation analytical approach of measuring four kinds of hydramine in the doctor solution simultaneously, may further comprise the steps:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, the eluent inflow conductance flow cell from chromatography column output is converted into electric signal by electric conductivity detector, is surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample gets into chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is imported in the chromatography column continuously, constantly hydramine and common kation are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppress electricity and lead check and analysis: during through 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 the formation spectrogram is by record.
Hydramine in the doctor solution of the present invention is isopropanolamine (IPA), and eluent is the 2.0mM crown ether, the 2.2mM pyrovinic acid, and 0.5mM L-histidine mixed solution adopts isocratic elution.
Hydramine in the doctor solution of the present invention is triisopropanolamine (TIPA), and eluent is the 2.0mM crown ether, the 2.2mM pyrovinic acid, and 0.5mM L-histidine mixed solution adopts isocratic elution.
Hydramine in the doctor solution of the present invention is N methyldiethanol amine (MDEA), and eluent is the 2.0mM crown ether, the 2.2mM pyrovinic acid, and 0.5mM L-histidine mixed solution adopts isocratic elution.
Hydramine in the doctor solution of the present invention is N, and N-dimethyl diethanolamine (DMAE), eluent are the 2.0mM crown ether, the 2.2mM pyrovinic acid, and 0.5mM L-histidine mixed solution adopts isocratic elution.
Separating column of the present invention is a TSK gelSuper IC-CR cation exchange column, and sample size is 30 μ L.
The present invention has following beneficial effect:
1. can carry out good compartment analysis to hydramine commonly used in four kinds of doctor solutions, the relative standard deviation of retention time, peak height, peak area is all less than 2%, and LDL 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. when analyzing, sample is directly injected the ion chromatographic separation post separate, suppress just can obtain spectrogram through electric conductivity detector afterwards, remove the step of deriving in the existing method, technological process is greatly simplified by suppressing glue;
3. this method can be used for the detection of the pure amine content in the practical sulphur removal technology.
Description of drawings
Fig. 1 is according to four kinds of hydramine and six kinds of cationic mixed standard solution chromatograms in the doctor solution of method acquisition provided by the invention; Among the 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 the middle hydramine chromatogram of actual sample doctor solution (lean solution) that obtains according to method provided by the invention, among the 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 specified:
Processing step comprises that successively mapping, sample introduction and ion-exchange, wash-out, non-system electricity lead check and analysis:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, the eluent inflow conductance flow cell from chromatography column output is converted into electric signal by electric conductivity detector, is surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample gets into chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is imported in the chromatography column continuously, constantly hydramine and common kation are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppress electricity and lead check and analysis: during through 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 the formation spectrogram is by record.
When analyzing above-mentioned alkanolamine solution, separating column is a TSK gelSuper IC-CR cation exchange column, and eluent is the 2.0mM crown ether, and 2.2mM pyrovinic acid, the mixed solution of 0.5mM L-histidine, sample size are 30 μ L, adopts isocratic elution.
Specify the present invention below in conjunction with accompanying drawing:
Embodiment:
Present embodiment is that the lean solution sample that contains desulfurizing agent in the 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, 3 μ m), kation suppresses glue (TOSOH); TSK gelSuper IC-CR cation exchange column, 30 μ L quantifying ring; Flow velocity: 1.0mL/min; Column temperature: 40 ℃; 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, the eluent inflow conductance flow cell from chromatography column output is converted into electric signal by electric conductivity detector, is surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample gets into chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is imported in the chromatography column continuously, constantly hydramine and common kation are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppress electricity and lead check and analysis: from the alkanolamine solution of chromatography column output by suppress glue suppress after during through conductance cell the process electric conductivity detector be converted into electric signal; Thereby form spectrogram by record, the Fig. 1 that is surveyed and drawn is according to four kinds of hydramine and six kinds of cationic mixed standard solution chromatograms in the doctor solution of method acquisition provided by the invention; Among the 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 the middle hydramine chromatogram of actual sample doctor solution (lean solution) that obtains according to method provided by the invention, among the figure, and 1=Na
+, 2=DMAE, 3=MDEA, 4=unkown, 5=NH
4 +, 6=Mg
2+, 7=Ca
2+, 8=K
+
Analysis result:
Through calculating, DMAE content is 6.6% in this lean solution, and MDEA content is 34.8%.TIPA and IPA do not detect, and DMAE and MDEA average recovery rate are respectively 103.15%, 95.48% in the sample, and the recovery of standard addition of TIPA and IPA is respectively 97.64%, 92.41%.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in spirit of the present invention and claim protection domain, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (6)
1. an ion chromatographic separation analytical approach of measuring four kinds of hydramine in the doctor solution simultaneously is characterized in that, may further comprise the steps:
(1) baseline mapping: make it reach balance with pump input chromatography column the eluent of mixed preparing, the eluent inflow conductance flow cell from chromatography column output is converted into electric signal by electric conductivity detector, is surveyed and drawn thereby form baseline;
(2) sample introduction and ion-exchange: tested sample gets into chromatography column and produces ion-exchange under the promotion of the eluent of mixed preparing;
(3) wash-out: eluent is imported in the chromatography column continuously, constantly hydramine and common kation are launched on chromatography column, each ion produces differential migration and is separated from each other, in different retention times by wash-out;
(4) suppress electricity and lead check and analysis: during through 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 the formation spectrogram is by record.
2. the ion chromatographic separation analytical approach of four kinds of hydramine is characterized in that in the doctor solution according to claim 1, and the hydramine in the described doctor solution is isopropanolamine (IPA); Eluent is the 2.0mM crown ether; 2.2mM pyrovinic acid, 0.5mM L-histidine mixed solution adopts isocratic elution.
3. the ion chromatographic separation analytical approach of four kinds of hydramine is characterized in that in the doctor solution according to claim 1, and the hydramine in the described doctor solution is triisopropanolamine (TIPA); Eluent is the 2.0mM crown ether; 2.2mM pyrovinic acid, 0.5mML-histidine mixed solution adopts isocratic elution.
4. the ion chromatographic separation analytical approach of four kinds of hydramine in the doctor solution according to claim 1; It is characterized in that; Hydramine in the described doctor solution is N methyldiethanol amine (MDEA), and eluent is the 2.0mM crown ether, the 2.2mM pyrovinic acid; 0.5mM L-histidine mixed solution adopts isocratic elution.
5. the ion chromatographic separation analytical approach of four kinds of hydramine in the doctor solution according to claim 1; It is characterized in that the hydramine in the described doctor solution is N, N-dimethyl diethanolamine (DMAE); Eluent is the 2.0mM crown ether; 2.2mM pyrovinic acid, 0.5mM L-histidine mixed solution adopts isocratic elution.
6. according to the ion chromatographic separation analytical approach of four kinds of hydramine in claim 1 or 2 or 3 or the 4 or 5 described doctor solutions, it is characterized in that described separating column is a TSK gelSuper IC-CR cation exchange column, sample size is 30 μ L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106442804A (en) * | 2016-11-23 | 2017-02-22 | 福建出入境检验检疫局检验检疫技术中心 | Detection method for migration quantity of alcamine substances in food plastic package bag |
| CN106918669A (en) * | 2017-02-21 | 2017-07-04 | 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 |
| CN111474249A (en) * | 2020-03-11 | 2020-07-31 | 台州学院 | Method for detecting organic alcohol amine compounds in environmental water sample |
| CN112781794A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Amine liquid water cooler leakage online monitoring method and system |
| CN112782288A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Separation detection method for amine and impurities in amine-containing aqueous solution |
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2012
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Non-Patent Citations (2)
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| 吴述超等: "电渗析离子交换-离子色谱法检测脱硫胺液中的热稳态盐", 《石油化工》 * |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106442804A (en) * | 2016-11-23 | 2017-02-22 | 福建出入境检验检疫局检验检疫技术中心 | Detection method for migration quantity of alcamine substances in food plastic package bag |
| 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 |
| CN106918669A (en) * | 2017-02-21 | 2017-07-04 | 华润水泥技术研发有限公司 | The detection method of alcohols, alcamine compound in grinding aid |
| 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 |
| CN112781794A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Amine liquid water cooler leakage online monitoring method and system |
| CN112782288A (en) * | 2019-11-06 | 2021-05-11 | 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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