CN103412084B - Method for determining effective substance content of petroleum sulfonate - Google Patents
Method for determining effective substance content of petroleum sulfonate Download PDFInfo
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- CN103412084B CN103412084B CN201310274591.7A CN201310274591A CN103412084B CN 103412084 B CN103412084 B CN 103412084B CN 201310274591 A CN201310274591 A CN 201310274591A CN 103412084 B CN103412084 B CN 103412084B
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Abstract
The invention relates to a method for determining the effective substance content of petroleum sulfonate, which comprises the following steps: weighing 0.5-1.0g of petroleum sulfonate; putting the petroleum sulfonate in a 25mL measuring flask, shaking up, and diluting to the specified volume, thus obtaining a detection sample; putting 1mL of detection sample in a 100mL measuring cylinder with a stopper, adding 5-8 drops of mixed indicator, 5-10 drops of thymol blue indicator and 5-10mL of sodium sulfate acidic solution, adding water to keep the water phase at 30-35mL, adding 15-20mL of dichloromethane, oscillating, and shaking up to obtain a mixed sample, wherein the mixed indicator is a mixture of methylene blue and methyl orange; titrating the mixed sample with a CTMAB (cetyl trimethyl ammonium bromide) solution until the titration end point (namely the bottom phase is changed from blue to green); and calculating the concentration of the sulfonate according to the titration result. The method has the advantages of high precision, simple and quick operation process, high reliability, clear end point and less interference.
Description
Technical field
The present invention relates to a kind of method measuring mahogany sulfonate working substance content, belong to petroleum exploration and development technical field.
Background technology
Because sulfonate surfactant is cheap, active efficiency is high, and working concentration is low, because of but adopt maximum surfactants in maximum, the research work of output up to now and site test.China has successively carried out ternary composite driving pilot test in the oil field such as grand celebration, triumph, achieves good effect.
Petroleum sulfonate surfactant has low interfacial tension, best phase and higher solubilising power, and raw material sources are extensive.Mahogany sulfonate occupies critical role in tertiary oil recovery, and it is very significant for setting up the fast and convenient method being applicable to petroleum sulfonate for tertiary oil recovery assay.The common method of current mensuration mahogany acid salt content has and generally adopts extraction, gravimetric method, membrane system method, titrimetry, high performance liquid chromatography, spectroscopic methodology etc. to purify to it at present and assay etc.Diphasic titration is adopted to measure petroleum sulfonate for tertiary oil recovery working substance content, simply, fast, in desk research and field test, widely use the method is that mahogany sulfonate uses tetravalence ammonium salt (hamming 1622) titration in rare sulfuric acid and chloroformic solution, and indicator used is the mixed indicator sold by the BOH laboratory of England.This indicator is expensive and at home market is not easily buied.And chloroform, to photaesthesia, meets illumination meeting and the oxygen effect in air, and decompose gradually and generate hypertoxic phosgene (phosgene) and hydrogen chloride, easy contaminated environment causes poisoning, harmful.In addition, when adopting hamming 1622 to carry out titration in prior art, reaction end not easily judges.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of method measuring mahogany sulfonate working substance content, with cetyl trimethyl ammonium bromide (CTMAB) solution for titrant, with methylene blue-methyl orange potpourri and thymol blue for indicator, adopt diphasic titration, measure the content of sulfonated bodies PetroChina Company Limited. sulfonate, have safe and efficient, titration end-point is feature clearly.
For achieving the above object, the invention provides a kind of method measuring mahogany sulfonate working substance content, it comprises the following steps:
Take 0.5-1.0g mahogany sulfonate, record its quality, to can be as accurate as after radix point four;
Mahogany sulfonate be placed in 25mL volumetric flask and shake up constant volume, obtaining detecting sample;
1mL is detected sample and be placed in 100mL tool plug graduated cylinder, add that 5-8 drips mixed indicator, 5-10 drips thymol blue indicator and 5-10mL sodium sulphate acid solution, add water and make aqueous phase keep 30-35mL, add 15-20mL methylene chloride, after vibration shakes up, obtain biased sample; Wherein, described mixed indicator is the potpourri of methylene blue and methyl orange;
By the titration of described recombined sample CTMAB solution, become green from blueness and be titration end-point down;
Calculate the concentration of sulfonate according to titration results, sulfonate content computing formula is:
In formula: N is the concentration of CTMAB solution, unit is mol/L;
V is the volume of the CTMAB solution consumed, and unit is mL;
M is the average molar mass of mahogany sulfonate, and unit is g/mol;
W is the quality of mahogany sulfonate, and unit is g.
Wherein, the average molar mass of mahogany sulfonate can get 370g/mol.
In the above-mentioned methods, preferably, mixed indicator is prepared by following steps:
Take methylene blue and methyl orange, wherein, the mass ratio of methylene blue and methyl orange is that 12:1-8:1(is preferably 10:1), the gross mass of methylene blue and methyl orange is 2-3g;
By methylene blue concentration be more than 90v% alcohol dissolve, methyl orange with hot water dissolving, then the two merging proceeded in 1L volumetric flask, be diluted with water to scale, obtain mixed indicator, wherein, the mass ratio of methylene blue and alcohol is 1:30-1:300.When the mass ratio of methylene blue and methyl orange is 10:1, be made into the mixed indicator containing 0.2wt% methylene blue and 0.02wt% methyl orange, dosage drips at 5-8, and add 5-10 when dripping thymol blue indicator, terminal colour change can be observed more significantly, its Variation Features is upper extremely blue, lower to blue to green by pink.
In the above-mentioned methods, preferably, mixed indicator, thymol blue indicator, sodium sulphate acid solution add successively.
In the above-mentioned methods, preferably, often liter of sodium sulphate acid solution contains the Na of 100g
2sO
4with the dense H that the concentration of 12.6mL is 98wt%
2sO
4, surplus is water.
In the above-mentioned methods, preferably, CTMAB solution is prepared by following steps:
Take the CTMAB of 0.3645g, dissolve with 200mL n-propanol and proceed to volumetric flask, adding water and be settled to 1000mL, obtain CTMAB solution;
With Sodium Tetraphenylborate Method, CTMAB solution is demarcated: take a certain amount of tetraphenylboron sodium in 100mL tool plug graduated cylinder, add 20mL phosphate buffer solution again, 20mL methylene chloride, 8 methylene blue-methyl orange potpourris make indicator, then the titration of CTMAB solution is used, separately do blank test, determined the concentration of CTMAB solution by titration results.
In the above-mentioned methods, preferably, phosphate buffer solution is prepared by following steps:
The sodium phosphate aqueous solution be sodium hydrogen phosphate aqueous solution and the 100mL concentration of 0.065mol/L by 300mL concentration being 0.065mol/L mixes, and obtains phosphate buffer solution.
In the above-mentioned methods, preferably, thymol blue indicator is prepared by following steps:
0.100g thymol blue being dissolved in 200mL concentration is in the ethanol water of 20v%, and filter after dissolving, filtrate water is diluted to 500mL, obtains thymol blue indicator.
The present invention adopts cheap methylene chloride, can avoid adopting chloroform easily to pollute and poisoning problem in prior art.Meanwhile, by adopting CTMAB, and adding mixed indicator and thymol blue can make drop reaction terminal more easily judge, overcoming the problem existing for prior art.
Method provided by the present invention adopts diphasic titration to measure mahogany sulfonate working substance content to have higher precision, easy and simple to handle, quick, reliability strong, and terminal is clear, disturb little, reagent is common reproducible, and its relative standard deviation is less than 1.0%, inorganic salts (Na in system
2sO
4, Na
2cO
3, NaCl) existence on measurement result without impact.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
Present embodiments provide the method measuring mahogany sulfonate working substance content, it comprises the following steps:
1, choose known working substance content be 90% neopelex test, accurately take neopelex 5.0000g, add in distilled water constant volume to the volumetric flask of 100mL to be measured, its theoretical working substance content is 4.5%.
2, get 50 milliliters of glass beakers 1, take liquid to be measured and be about 0.8342g(W).
3,0.8342g sample is placed in 25mL volumetric flask, adding distil water shakes up constant volume, get 1mL sample with transfer pipet and be placed in 100mL tool plug graduated cylinder, add 5 mixed indicators successively, 5-10 drips thymol blue indicator and 5mL sodium sulphate acid solution (often liter of sodium sulphate acid solution contains the Na of 100g
2sO
4with the dense H that the concentration of 12.6mL is 98wt%
2sO
4, surplus is water), add water and make aqueous phase keep 30mL, add methylene chloride 15mL, obtains recombined sample after vibration shakes up, for subsequent use.
Wherein, mixed indicator is prepared by following steps:
Take methylene blue and methyl orange, the mass ratio of methylene blue and methyl orange is 10:1, and the gross mass of methylene blue and methyl orange is 2.2g;
By methylene blue concentration be 95v% alcohol dissolve, methyl orange with hot water dissolving, then the two merging proceeded in 1L volumetric flask, be diluted with water to scale, obtain mixed indicator, wherein, the mass ratio of methylene blue and alcohol is 1:200;
0.100g thymol blue being dissolved in 200mL concentration is in the ethanol water of 20v%, and filter after dissolving, filtrate water is diluted to 500mL, obtains thymol blue indicator.
3, be 0.00101mol/L(N by recombined sample concentration) the titration of CTMAB solution, be titration end-point by blue to green down, consume CTMAB solution 4.23mL(V), calculate the concentration of sulfonate according to titration results.
Wherein, CTMAB solution is prepared by following steps:
Take the CTMAB of 0.3645g, dissolve with 200mL n-propanol and proceed to volumetric flask, adding water and be settled to 1000mL, obtain CTMAB solution;
Take 1g tetraphenylboron sodium in 100mL tool plug graduated cylinder, add 20mL phosphate buffer solution and 20mL methylene chloride again, 8 methylene blue-methyl orange potpourris make indicator, then the titration of CTMAB solution is used, separately do blank test, determine that the concentration of CTMAB solution is 0.00101mol/L by titration results.
4, sulfonate content computing formula is:
Wherein, M is the average molar mass of mahogany sulfonate, gets 348.48g/mol.
Difference between above-mentioned test result and theoretical working substance content is 0.04%, and error rate is only 0.04/4.5 × 100%=0.9%.Can find out according to the above results, the method of mensuration mahogany sulfonate working substance content provided by the present invention can measure mahogany sulfonate working substance content exactly, and the method has higher precision, easy and simple to handle, quick, reliability is strong, terminal is clear, disturbs little.
Claims (6)
1. measure a method for mahogany sulfonate working substance content, it comprises the following steps:
Take 0.5-1.0g mahogany sulfonate, record its quality;
Mahogany sulfonate be placed in 25mL volumetric flask and shake up constant volume, obtaining detecting sample;
1mL is detected sample and be placed in 100mL tool plug graduated cylinder, add that 5-8 drips mixed indicator, 5-10 drips thymol blue indicator and 5-10mL sodium sulphate acid solution, add water and make aqueous phase keep 30-35mL, add 15-20mL methylene chloride, after vibration shakes up, obtain biased sample; Wherein, described mixed indicator is the potpourri of methylene blue and methyl orange;
By the titration of described recombined sample CTMAB solution, become green from blueness and be titration end-point down;
Calculate the concentration of sulfonate according to titration results, sulfonate content computing formula is:
In formula: N is the concentration of CTMAB solution, unit is mol/L;
V is the volume of the CTMAB solution consumed, and unit is mL;
M is the average molar mass of mahogany sulfonate, and unit is g/mol;
W is the quality of mahogany sulfonate, and unit is g;
Wherein, described mixed indicator is prepared by following steps:
Take methylene blue and methyl orange, wherein, the mass ratio of methylene blue and methyl orange is 12:1-8:1, and the gross mass of methylene blue and methyl orange is 2-3g;
By methylene blue concentration be that the alcohol of more than 90v% dissolves, methyl orange is with hot water dissolving, then the two merging is proceeded in 1L volumetric flask, be diluted with water to scale, obtain described mixed indicator, wherein, the mass ratio of described methylene blue and alcohol is 1:30-1:300.
2. method according to claim 1, wherein, the mass ratio of described methylene blue and methyl orange is 10:1.
3. method according to claim 1, wherein, often liter of described sodium sulphate acid solution contains the Na of 100g
2sO
4with the dense H that the concentration of 12.6mL is 98wt%
2sO
4, surplus is water.
4. method according to claim 1, wherein, described CTMAB solution is prepared by following steps:
Take the CTMAB of 0.3645g, dissolve with 200mL n-propanol and proceed to volumetric flask, adding water and be settled to 1000mL, obtain CTMAB solution;
Take a certain amount of tetraphenylboron sodium in 100mL tool plug graduated cylinder, then add 20mL phosphate buffer solution, 20mL methylene chloride, 8 methylene blue-methyl orange potpourris make indicator, then use the titration of CTMAB solution, separately do blank test, determined the concentration of CTMAB solution by titration results.
5. method according to claim 4, wherein, described phosphate buffer solution is prepared by following steps:
The sodium phosphate aqueous solution be sodium hydrogen phosphate aqueous solution and the 100mL concentration of 0.065mol/L by 300mL concentration being 0.065mol/L mixes, and obtains described phosphate buffer solution.
6. method according to claim 1, wherein, described thymol blue indicator is prepared by following steps:
0.100g thymol blue being dissolved in 200mL concentration is in the ethanol water of 20v%, and filter after dissolving, filtrate water is diluted to 500mL, obtains described thymol blue indicator.
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中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.表面活性剂 工业烷烃磺酸盐烷烃单磺酸盐含量的测定(直接两相滴定法).《中 华 人 民 共 和 国 国 家 标 准EN/T20199-2006》.2006, * |
亚甲基蓝-甲基橙混合指示剂测定三次采油用石油磺酸盐有效物含量;李柏林等;《大庆石油地质与开发》;20040630;第23卷(第3期);第75-76页 * |
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