CN103134792A - Method for determining manganese element in ethanol gasoline - Google Patents
Method for determining manganese element in ethanol gasoline Download PDFInfo
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- CN103134792A CN103134792A CN2011103802763A CN201110380276A CN103134792A CN 103134792 A CN103134792 A CN 103134792A CN 2011103802763 A CN2011103802763 A CN 2011103802763A CN 201110380276 A CN201110380276 A CN 201110380276A CN 103134792 A CN103134792 A CN 103134792A
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Abstract
The invention relates to a method for determining manganese element in ethanol gasoline. The method comprises: diluting an inorganic manganese solution sequentially by using absolute alcohol and gasoline to prepare 3-5 water-ethanol-gasoline system manganese standard solutions with a concentration of 0-20 mg/L; sequentially spraying the manganese standard solutions with the different concentrations into an inductively coupled plasma atomic emission spectrometer to respectively determine emission intensities; drawing a standard work curve according a relationship between the concentration in the solution and the emission intensity; and sequentially spraying ethanol gasoline samples requiring determination into the inductively coupled plasma atomic emission spectrometer to respectively determine emission intensities, and calculating manganese element contents in the samples requiring determination according to the drawn standard work curve. With the method, the sample pretreatment is not required, analysis is rapid, and the result is accurate.
Description
Technical field
The invention belongs to the assay method of metallic element in a kind of petroleum products, more particularly, relate to a kind of method of measuring manganese element in ethanol petrol.
Background technology
Constantly reduce at world petroleum resource, in the increasingly severe situation of world energy sources situation, the new energy, particularly regenerative resource are being sought and developed in each state all.From the eighties of last century later stage, the countries such as the U.S., Brazil just take the lead in ethanol is used as vehicle fuel.China uses in beginning pilot conversion in 2002 vehicle-use alcohol gasoline (being E10 gasoline) that contains ethanol 10% (V/V).The vehicle-use alcohol gasoline that uses in the market is to form with absolute ethyl alcohol and the gasoline component mediation of liquid water content less than 0.2% (V/V).
Compare with traditional motor petrol, the vehicle-use alcohol gasoline cleaning capacity is stronger, easily the impurity on container inner wall is washed down, in gasoline, metallic element such as manganese etc. will increase like this, will certainly have influence on the usability of engine, therefore, be necessary to measure quickly and accurately manganese content in ethanol petrol.
The method of measuring at present metallic element in gasoline is that sample to be tested and organic solvent (as methyl isobutyl ketone etc.) are mixed, and employing atomic absorption spectrum (AAS) is measured (SH/T0711-2002).The method in use will contact a large amount of organic solvents, and toxicity is larger; Sample needs further to process, and operates comparatively loaded down with trivial details.
Summary of the invention
The purpose of this invention is to provide a kind of method of measuring manganese element in ethanol petrol, to measure quickly and accurately the manganese element in vehicle-use alcohol gasoline.
In mensuration ethanol petrol provided by the invention, the method for manganese element comprises the following steps:
(1) preparation of standard solution: inorganic manganese solution successively with the dilution of absolute ethyl alcohol, gasoline, is mixed with concentration and is 3～5 water-ethanols of 0～20mg/L-gasoline system manganese standard solution; Water-ethanol-gasoline volume ratio is 0.4: 9.6: 90;
(2) test of standard solution: the manganese standard solution of various concentration in step (1) is sprayed into inductively coupled plasma atomic emission spectrometer (ICP/AES) successively test respectively its emissive porwer, and concern the drawing standard working curve according to concentration in solution and emissive porwer;
(3) test of sample to be tested: ethanol petrol sample to be measured is sprayed into inductively coupled plasma atomic emission spectrometer (ICP/AES) successively test respectively its emissive porwer, and according to the standard working curve of drawing in step (2), draw the manganese element content in sample to be tested.
Inorganic manganese solution of the present invention is four water manganous chloride (MnCl
24H
2O) acid solution, in described acid solution, acid is 0.1～10: 1 with the volume ratio of water, described acid is hydrochloric acid or nitric acid.
Absolute ethyl alcohol liquid water content of the present invention is less than 0.2% (V/V).
Described gasoline component is selected from one or more in hydrotreated naphtha, catalytically cracked gasoline, catalytic reforming (CR) gasoline, straight-run gasoline, alkylate oil, isomerization gasoline, etherified gasoline.
This method is to adopt inductively coupled plasma atomic emission spectrometer (ICP/AES) that the manganese content in industrial alcohol gasoline is measured.
ICP/AES Instrument operation parameter setting range is as follows:
Power 1.40kW～1.50kW,
Plasma gas flow rate 16L/min～17L/min,
Assisted gas flow 0.8L/min～1.5L/min,
Atomization gas flow 0.5L/min～1.0L/min,
Pump speed 0.6L/min～1.0L/min.
Plasma (orifice) gas, assisted gas, atomization gas and carrier gas are argon gas.
Adopt inorganic manganese standard solution, absolute ethyl alcohol to be mixed with the matrix standard solution consistent with sample to be tested with gasoline component, sample need not can directly measure through processing.
Compared with prior art, method advantage of the present invention is as follows:
(1) this method need not sample is carried out pre-service, and analysis speed is fast;
(2) do not need dilution due to sample in the mensuration process, therefore can not reduce emissive porwer, result is more accurate;
(3) method only uses a small amount of absolute ethyl alcohol and component gasoline in the standard preparation process, and can not use a large amount of organic solvents such as methyl isobutyl ketone, and operating process is safer, and toxicity is less.
Description of drawings
Fig. 1 manganese element concentration and emissive porwer concern standard working curve.
Embodiment
Embodiment of the present invention ICP/AES instrument used model is Optima 5300V, is made by German PerkinElmer (PE) Instr Ltd..ICP/AES Instrument operation parameter setting value is as follows:
Power 1.45kW,
Plasma gas flow rate 17L/min,
Assisted gas flow 1.5L/min,
Atomization gas flow 0.5L/min,
Pump speed 0.5L/min.
Plasma (orifice) gas, assisted gas, atomization gas and carrier gas are argon gas.
Take the four water manganous chloride (MnCl of 345.54mg
24H
2O) in clean beaker, add deionized water, after four water manganous chloride all dissolve, quantitatively be transferred in the 100mL volumetric flask, be diluted with water to scale, shaking up and making concentration is that 1000mg/L is to the manganese standard solution.
Get three 50ml volumetric flasks, pipetting respectively concentration is manganese standard solution 0ml, 0.5ml and the 1.0ml of 1000mg/L, is diluted to scale with absolute ethyl alcohol, and being mixed with concentration is the manganese standard solution of 0mg/L, 10mg/L, 20mg/L.
Separately get the volumetric flask of three 50ml, pipetting respectively concentration is 0mg/L, 10mg/L and each 5ml of 20mg/L manganese standard solution, is diluted to scale with gasoline component (catalytically cracked gasoline and catalytic reforming (CR) gasoline volume ratio are 3: 1), shakes up.Be mixed with concentration and be the water-ethanol of 0mg/L, 1.0mg/L, 2.0mg/L-gasoline system manganese standard solution.
Spraying into successively concentration is 0mg/L, 1.0mg/L, 2.0mg/L manganese standard solution, and the drawing standard working curve, as shown in drawings.In standard solution, manganese element is in the scanning at 238.204nm place, the standard working curve of drawing according to the relation of concentration and emissive porwer in its solution, it is y=0.001x (in formula, y is manganese element concentration in sample to be tested, and x is the emissive porwer of manganese element in sample to be tested) that match obtains linear relation.
The below will investigate detection limit, interference, the recovery and the repeatability of the inventive method.
1, method detection limit
With 10 blank solutions of building standard working curve METHOD FOR CONTINUOUS DETERMINATION, calculate the standard deviation of three times as the detection limit of the method, Mn 257.61nm detects and is limited to 0.00324.Test figure sees Table 1.
Table 1 detection limit
2, interference test
This method is used for measuring ethanol petrol manganese element content.Because metal element content in sample is all very low, might introduce sample to be tested at home and abroad in transportation, storage and transport process except manganese element, other element does not almost have the possibility of introducing, does not have disturbing effect between element.
3, the recovery test of method
The assay method recovery that increases the weight of to reclaim is adopted in this test.Add the manganese standard solution that adds respectively 0.5mg/L and 1.0mg/L in the sample of 0.5mg/L and 1.0mg/L in sample, measure total manganese content and calculate recovery rate in sample, test sees Table 2.The recovery of this method is between 98%～102%.
The recovery test of table 2 method
| Specimen coding | Measured value | The standard addition | Measure total amount | The |
| 1 | 0.5 | 0.50 | 1.00 | 100％ |
| 2 | 0.5 | 1.0 | 1.49 | 98％ |
| 3 | 1.0 | 0.50 | 1.51 | 101％ |
| 4 | 1.0 | 1.0 | 2.02 | 102％ |
Can find out from the data of table 2, during at 1mg/L～5mg/L, the recovery of method is 90%～110% when the concentration of manganese element in sample, and the sample this method that exceeds this scope is tested.It can also be seen that from table 2 data, along with the increase of concentration of element, the recovery of method is become better and better.
4, the replica test of method
Three ethanol petrol standard samples have been prepared in this test, within the different time, these three samples are carried out repeatedly replication, the relative standard deviation of result of calculation.Test findings sees Table 3.
The repeated experiment of table 3 method
| Specimen coding | Measured value | Number of times | RSD％ |
| 1 | 0.5 | 9 | 9.37 |
| 2 | 1.0 | 9 | 7.25 |
| 3 | 2.0 | 9 | 4.39 |
Can find out from the data of table 3, the relative standard deviation of method (RSD) is less than 10%, and along with the increase of manganese element concentration in sample, the relative standard deviation of result reduces gradually, and the repeatability of method is become better and better.
Claims (7)
1. method of measuring manganese element in ethanol petrol, it is characterized in that: the method comprises the following steps:
(1) preparation of standard solution: inorganic manganese solution successively with the dilution of absolute ethyl alcohol, gasoline, is mixed with concentration and is 3～5 water-ethanols of 0～20mg/L-gasoline system manganese standard solution; Water, ethanol, gasoline volume ratio are 0.4: 9.6: 90;
(2) test of standard solution: the manganese standard solution of various concentration in step (1) is sprayed into inductively coupled plasma atomic emission spectrometer successively test respectively its emissive porwer, and concern the drawing standard working curve according to concentration in solution and emissive porwer;
(3) test of sample to be tested: ethanol petrol sample to be measured is sprayed into inductively coupled plasma atomic emission spectrometer successively test respectively its emissive porwer, and the standard working curve drawn middle according to step (2) draws the manganese element content in sample to be tested.
2. according to the method for claim 1, it is characterized in that: described inorganic manganese solution is the acid solution of four water manganous chloride.
3. according to the method for claim 2, it is characterized in that: in described acid solution, acid is 0.1～10: 1 with the volume ratio of water.
4. according to the method for claim 2 or 3, it is characterized in that: described acid is hydrochloric acid or nitric acid.
5. according to the method for claim 1, it is characterized in that: described absolute ethyl alcohol liquid water content is less than 0.2V%.
6. according to the method for claim 1, it is characterized in that: described gasoline component is selected from one or more in hydrotreated naphtha, catalytically cracked gasoline, catalytic reforming (CR) gasoline, straight-run gasoline, alkylate oil, isomerization gasoline, etherified gasoline.
7. according to the method for claim 1, it is characterized in that: inductively coupled plasma atomic emission spectrometer operating parameter setting range is as follows:
Power 1.40kW～1.50kW,
Plasma gas flow rate 16L/min～18L/min,
Assisted gas flow 0.8L/min～1.5L/min,
Atomization gas flow 0.5L/min～1.0L/min,
Pump speed 0.6L/min～1.0L/min,
Plasma (orifice) gas, assisted gas, atomization gas and carrier gas are argon gas.
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| CN2011103802763A CN103134792A (en) | 2011-11-25 | 2011-11-25 | Method for determining manganese element in ethanol gasoline |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108645810A (en) * | 2018-04-03 | 2018-10-12 | 成都产品质量检验研究院有限责任公司 | The precious good and bad rapid detection method of polyisobutene amine fuel oil |
| CN114487077A (en) * | 2020-11-12 | 2022-05-13 | 中国石油天然气股份有限公司 | Method for measuring arsenic content in diesel oil |
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| US6686999B2 (en) * | 2001-12-14 | 2004-02-03 | Air Products And Chemicals, Inc. | Method of using an aerosol to calibrate spectrometers |
| JP2008070225A (en) * | 2006-09-14 | 2008-03-27 | Matsushita Electric Ind Co Ltd | Element concentration analysis method of electroless nickel plating |
| JP2010002371A (en) * | 2008-06-23 | 2010-01-07 | Toppan Printing Co Ltd | Analysis method of element component in liquid sample |
| CN101349648A (en) * | 2008-07-17 | 2009-01-21 | 武汉钢铁(集团)公司 | Method for measuring trace elements in high titanium high boiler slag |
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| CN108645810A (en) * | 2018-04-03 | 2018-10-12 | 成都产品质量检验研究院有限责任公司 | The precious good and bad rapid detection method of polyisobutene amine fuel oil |
| CN108645810B (en) * | 2018-04-03 | 2021-06-08 | 四川省产品质量监督检验检测院 | Method for rapidly detecting quality of polyisobutene amine fuel |
| CN114487077A (en) * | 2020-11-12 | 2022-05-13 | 中国石油天然气股份有限公司 | Method for measuring arsenic content in diesel oil |
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Application publication date: 20130605 |