CN103389327A - Method for testing organochlorine content of oil extraction auxiliary agent - Google Patents
Method for testing organochlorine content of oil extraction auxiliary agent Download PDFInfo
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- CN103389327A CN103389327A CN201210138619XA CN201210138619A CN103389327A CN 103389327 A CN103389327 A CN 103389327A CN 201210138619X A CN201210138619X A CN 201210138619XA CN 201210138619 A CN201210138619 A CN 201210138619A CN 103389327 A CN103389327 A CN 103389327A
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Abstract
The invention provides a method for testing organochlorine content of an oil extraction auxiliary agent. The method is as below: subjecting a sample to oxygen bottle combustion decomposition to convert organic chlorine into inorganic chlorine; absorbing by a NaOH solution; determining a total content by a salt content determinator; and subtracting the inorganic chlorine to obtain the organochlorine content of the oil extraction auxiliary agent. The invention realizes scientific and accurate usage and detection of oil extraction auxiliary agent for oil fields, effectively enhances product quality control level, actively promotes quality control on oil field products and material purchasing, and plays an important role for later crude oil processing, stabilization operation of oil refining apparatuses, equipment corrosion reduction and product quality improvement.
Description
Technical field
The present invention relates to the oil extraction in oil field auxiliary agent, more particularly relate to content of organic chloride method of testing in a kind of oil recovery auxiliary agent.
Background technology
At present, oil extraction in oil field auxiliary agent use amount is large, and is of a great variety, there is no the method for testing of the general content of organic chloride of science.Because the content of organic chloride in the oil recovery auxiliary agent can't directly be measured, after must first being converted into inorganic chlorine to the organochlorine in auxiliary agent, first measuring the content of total chlorine, then measure content of inorganic chlorine, always chlorine deducts inorganic chlorine and is content of organic chloride in medicament.Therefore whether the method for transformation of organochlorine and conversion are most important key problem in technology fully.Consult and experiment is groped by pertinent literature, the organochlorine method for transformation mainly contains several modes: halogenated hydrocarbons elimination method, alkaline water solution, the direct firing method of microcoulomb and oxygen firing method.
1) halogenated hydrocarbons elimination method
In the alcoholic solution of NaOH by elimination reaction (not all halogenated hydrocarbons can occur), slough one or several HX from two adjacent carbon on carbon skeleton, then with reaction NaOH, generate NaX, change organochlorine into inorganic chlorine, form simultaneously unsaturated link, obtain alkene or alkynes.With extraction, water oil two is separated again, measures the content of total chlorine, then deduct inorganic chlorine, be the content of organic chloride in the use chemical agent of oil field.Because the organochlorine composition and structure in most of chemical agent is unknown, the method has significant limitation, and for the halogenated hydrocarbons that can carry out elimination reaction, the organochlorine conversion ratio is also lower.
2) alkaline water solution
Halogenated hydrocarbons generation substitution reaction, be converted into alcohol in NaOH solution, and organochlorine is converted into inorganic chlorine simultaneously.Measure the content of total chlorine, then deduct inorganic chlorine, be the content of organic chloride in the use chemical agent of oil field.
Just there is certain feasibility in theory in the alkaline water solution, but the method can't operate in actual experiment.Reason is that hydrolysis reaction is a reversible reaction, in order to make hydrolysis, adds AgNO fully in reaction solution
3, the Cl-of hydrolysis is precipitated out with the form of AgCl, reaction is constantly carried out to positive dirction.But introduce AgNO
3Very easily generate the AgOH precipitation under alkali condition, can make measurement result bigger than normal.(dissolving of AgCl is long-pending is 1.8 * 10-10, and the dissolving of AgOH long-pending be 2.0 * 10-8).And AgOH is unstable, easily resolves into the silver oxide Ag of brown
2O, solution becomes pitchy, for the judgement of drop reaction terminal, has huge interference.
3) the direct firing method of microcoulomb
Directly reactant is injected in quartz ampoule with micro syringe, at high temperature burning, products of combustion passes through N
2And O
2Mixed gas bring in titration cell, measure the content of total chlorine.The method can directly be measured the content of total chlorine, but can't measure the content of inorganic chlorine.If adopt the salt content analyzer to measure organochlorine, two kinds of instruments are measured respectively total chlorine and content of inorganic chlorine, and assay method is infeasible.
4) oxygen firing method
Sample changes organochlorine into inorganic chlorine after the direct combustion decomposition of oxygen Molotov cocktail, after absorbing by NaOH solution, directly with the salt content analyzer, measure chloride content, then deduct the content of inorganic chlorine of mensuration, is the content of organic chloride in the use chemical agent of oil field.The standard specimen recovery of the method is more than 90%.
Summary of the invention
Purpose of the present invention is intended to overcome the deficiencies in the prior art, provides a kind of making use and detect the oil extraction in oil field auxiliary agent science is accurate more, content of organic chloride method of testing in the oil recovery auxiliary agent that the production quality control level effectively improves.
Purpose of the present invention can be achieved by the following technical measures:
This method of testing is carried out as follows:
A. the mensuration of chloride content:
a
1.Cut two onesize template flags, at an absorbent cotton that is used for the placement 0.04-0.06g of template flag central authorities of sample, roll on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar with the template flag, drip sample with the 1mL syringe on absorbent cotton, oil base sample sample weighting amount 0.05～0.10g, water base sample sample weighting amount is at 0.02～0.05g, and recording its quality is m
1Another is used for blank template flag and only places the consistent absorbent cotton of absorbent cotton that uses with sample;
a
2.Adding mass concentration in the oxygen Molotov cocktail is 28～32% hydrogen peroxide and each 2mL of NaOH of 0.08～0.12mol/L;
a
3.Pass into oxygen in the oxygen Molotov cocktail, time 1.5～2.5min, insert bottleneck with bottle stopper after then lighting the perfect combustion of template flag, will be inclined upwardly at the bottom of the oxygen Molotov cocktail, makes absorption liquid seal bottleneck; Jog oxygen Molotov cocktail after burning finishes, make the wetting bottle of absorption liquid wall, is placed to white cigarette and disappears;
a
4.Rinse oxygen Molotov cocktail wall and support bar three times with distillation moisture, then move to constant volume in the 100mL volumetric flask;
a
5. open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion at 80%-100%, then with microsyringe, adds the 1.4mL sample solution to measure total chlorine ion concentration X in electrolytic cell
1
a
6. do blank test with above same method, record the concentration X of chlorion in blank
01
a
7. chloride content is calculated as follows:
In formula:
A Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g;
B. the mensuration of content of inorganic chlorine:
b
1.Add sample consistent while with total chlorine, testing in the 100mL volumetric flask, recording its quality is m
2, water-soluble sample adds the distilled water constant volume, and the oil-soluble sample adds 95% ethanol constant volume, mixes;
b
2.By above-mentioned a
5Step is tested, and records inorganic chlorine ion concentration X in sample
2
b
3.With the salt content analyser, distilled water or 95% ethanol are carried out blank test, record chlorine ion concentration X in blank
02
b
4.Content of inorganic chlorine is calculated as follows:
In formula:
A Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g;
C. content of organic chloride %=
A Always-
A Nothing.
The present invention is when the mensuration of chloride content, if having black residue in oxygen Molotov cocktail absorption liquid, the interpret sample incomplete combustion, rekindle after should suitably reducing sample weighting amount.Each test all should be carried out blank test, and the blank value substitution is calculated.Paper flag, degreasing Cottonopolis blank and that sample uses should be clean, and uniform quality, make blank value as far as possible little.Measured value is higher, measures after should suitably reducing sample weighting amount or corresponding dilute sample when the tack peak appears in instrument again.Repetition measurement standard specimen once again after working sample finishes, to determine accuracy and the stationarity of instrument.
Salt content analyzer test Cl
-Principle: the sample after processing injects the acetic acid electrolytic solution that contains a certain amount of silver ion, and the chlorion in sample namely reacts with silver ion:
Cl
-+Ag
+ AgCl
The silver ion that reaction consumes is given birth to and is supplemented by the generating electrodes electricity, by measuring electricity, gives birth to the electric weight that silver ion consumes, and according to Faraday's law, can try to achieve chloride ion content.
This method Cl
-Detection limit: 0.5 mg/L～5000 mg/L, higher than can testing after Sample Dilution of the upper limit.
When the present invention tests content of organic chloride in the low oil recovery auxiliary agent of volatility, with quantitative filter paper, replace the template flag.
If the present invention uses the template flag, at a
4Adding mass concentration in absorption liquid after the step constant volume is that 0.18～0.22% barium nitrate l mL shelters again.
The present invention has formulated scientific and rational assay method for the content of organic chloride in test oil recovery auxiliary agent.The application of present technique, make and use and detect the oil extraction in oil field auxiliary agent science is accurate more, the production quality control level has obtained effective raising, the product quality in oil field and purchase of goods and materials quality control are played positive impetus and to the crude oil processing in later stage, the stable operation of oil refining apparatus, reduce equipment corrosion, improving the quality of products has important effect.
Description of drawings
Fig. 1 is the schematic diagram of template flag;
Fig. 2 is the structural representation of oxygen Molotov cocktail.
Embodiment
Embodiment 1:
This method of testing is carried out as follows:
A. the mensuration of chloride content:
a
1.Cut two onesize template flags according to Fig. 1, one is used for blank, and one is used for sample.At an absorbent cotton that is used for the placement 0.04g of template flag central authorities of sample, roll on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar with the template flag, drip sample with the 1mL syringe on absorbent cotton, oil base sample sample weighting amount is advisable at 0.10g, water base sample sample weighting amount is at 0.02g, accurately to 0.0001 g, recording its quality is m
1Another is used for blank template flag and only places the absorbent cotton of 0.04g, and sample should be tried one's best consistent with blank absorbent cotton quality, the size of using.The medicament that volatility is low can replace the template flag with quantitative filter paper;
a
2.Adding mass concentration in the oxygen Molotov cocktail is 32% hydrogen peroxide and each 2mL of NaOH of 0.08mol/L;
a
3.Pass into oxygen with suitable flow velocity (liquid level is the microwaviness shape) in the oxygen Molotov cocktail, time 2.5min, then hold on the other hand the oxygen Molotov cocktail, another hand is picked up bottle stopper and light the template flag on spirit lamp, rapidly bottle stopper is carefully inserted bottleneck, build bottle stopper, withstand bottle stopper with hand and be inclined upwardly at the bottom of with the oxygen Molotov cocktail, make absorption liquid seal bottleneck.After all burnt was slightly cooling, jog oxygen Molotov cocktail several times, made the wetting bottle of absorption liquid wall, then is placed to white cigarette and disappears, and generally needs 30 min;
a
4.Rinse oxygen Molotov cocktail wall and steady arm three times with distillation moisture, then move to constant volume in 100 mL volumetric flasks.If use the template flag, adding massfraction in absorption liquid is 0.22% barium nitrate l mL again, shelters the SO that the template flag is introduced
4 2-To Ag
+Interference.Can add barium nitrate while with quantitative filter paper, burning shelters; The covering method of other interfering ion is seen appendix 1;
a
5. open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion and is advisable between 80%-100%, then with microsyringe, adds the 1.4mL sample solution to measure total chlorine ion concentration X in electrolytic cell
1
a
6. do blank test with above same method, record the concentration X of chlorion in blank
01
a
7. chloride content is calculated as follows:
In formula:
A Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g;
B. the mensuration of described content of inorganic chlorine:
b
1.Add sample consistent while with total chlorine, testing in the 100mL volumetric flask, accurately to 0.0001 g, recording its quality after weighing is m
2, water-soluble sample adds the distilled water constant volume, and the oil-soluble sample adds 95% ethanol constant volume, mixes;
b
2.By above-mentioned a
5Step is tested, and records inorganic chlorine ion concentration X in sample
2
b
3.With the salt content analyser, distilled water or 95% ethanol are carried out blank test, record chlorine ion concentration X in blank
02
b
4.Content of inorganic chlorine is calculated as follows:
In formula:
A Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g;
C. content of organic chloride %=
A Always-
A Nothing.
Embodiment 2:
This method of testing is carried out as follows:
A. the mensuration of chloride content:
a
1.Cut two onesize template flags according to Fig. 1, one is used for blank, and one is used for sample.At an absorbent cotton that is used for the placement 0.06g of template flag central authorities of sample, roll on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar with the template flag, drip sample with the 1mL syringe on absorbent cotton, oil base sample sample weighting amount is advisable at 0.05g, water base sample sample weighting amount is at 0.05g, accurately to 0.0001 g, recording its quality is m
1Another is used for blank template flag and only places the absorbent cotton of 0.06g, and sample should be tried one's best consistent with blank absorbent cotton quality, the size of using.The medicament that volatility is low can replace the template flag with quantitative filter paper;
a
2.Adding mass concentration in the oxygen Molotov cocktail is 28% hydrogen peroxide and each 2mL of NaOH of 0.12mol/L;
a
3.Pass into oxygen with suitable flow velocity (liquid level is the microwaviness shape) in the oxygen Molotov cocktail, time 1.5min, then hold on the other hand the oxygen Molotov cocktail, another hand is picked up bottle stopper and light the template flag on spirit lamp, rapidly bottle stopper is carefully inserted bottleneck, build bottle stopper, withstand bottle stopper with hand and be inclined upwardly at the bottom of with the oxygen Molotov cocktail, make absorption liquid seal bottleneck.After all burnt was slightly cooling, jog oxygen Molotov cocktail several times, made the wetting bottle of absorption liquid wall, then is placed to white cigarette and disappears, and generally needs 30 min;
a
4.Rinse oxygen Molotov cocktail wall and steady arm three times with distillation moisture, then move to constant volume in 100 mL volumetric flasks.If use the template flag, adding massfraction in absorption liquid is 0.18% barium nitrate l mL again, shelters the SO that the template flag is introduced
4 2-To Ag
+Interference.Can add barium nitrate while with quantitative filter paper, burning shelters; The covering method of other interfering ion is seen appendix 1;
a
5. open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion and is advisable between 80%-100%, then with microsyringe, adds the 1.4mL sample solution to measure total chlorine ion concentration X in electrolytic cell
1
a
6. do blank test with above same method, record the concentration X of chlorion in blank
01
a
7. chloride content is calculated as follows:
In formula:
A Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g;
B. the mensuration of content of inorganic chlorine:
b
1.Add sample consistent while with total chlorine, testing in the 100mL volumetric flask, recording its quality is m
2, water-soluble sample adds the distilled water constant volume, and the oil-soluble sample adds 95% ethanol constant volume, mixes;
b
2.By above-mentioned a
5Step is tested, and records inorganic chlorine ion concentration X in sample
2
b
3.With the salt content analyser, distilled water or 95% ethanol are carried out blank test, record chlorine ion concentration X in blank
02
b
4.Content of inorganic chlorine is calculated as follows:
In formula:
A Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g;
C. content of organic chloride %=
A Always-
A Nothing.
Embodiment 3:
This method of testing is carried out as follows:
A. the mensuration of chloride content:
a
1.Cut two onesize template flags according to Fig. 1, one is used for blank, and one is used for sample.At an absorbent cotton that is used for the placement 0.04g of template flag central authorities of sample, roll on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar with the template flag, drip sample with the 1mL syringe on absorbent cotton, oil base sample sample weighting amount is advisable at 0.10g, water base sample sample weighting amount is at 0.02g, accurately to 0.0001 g, recording its quality is m
1Another is used for blank template flag and only places the absorbent cotton of 0.04g, and sample should be tried one's best consistent with blank absorbent cotton quality, the size of using.The medicament that volatility is low can replace the template flag with quantitative filter paper;
a
2.Adding mass concentration in the oxygen Molotov cocktail is 32% hydrogen peroxide and each 2mL of NaOH of 0.08mol/L;
a
3.Pass into oxygen with suitable flow velocity (liquid level is the microwaviness shape) in the oxygen Molotov cocktail, time 2.5min, then hold on the other hand the oxygen Molotov cocktail, another hand is picked up bottle stopper and light the template flag on spirit lamp, rapidly bottle stopper is carefully inserted bottleneck, build bottle stopper, withstand bottle stopper with hand and be inclined upwardly at the bottom of with the oxygen Molotov cocktail, make absorption liquid seal bottleneck.After all burnt was slightly cooling, jog oxygen Molotov cocktail several times, made the wetting bottle of absorption liquid wall, then is placed to white cigarette and disappears, and generally needs 30 min;
a
4.Rinse oxygen Molotov cocktail wall and steady arm three times with distillation moisture, then move to constant volume in 100 mL volumetric flasks.If use the template flag, adding massfraction in absorption liquid is 0.22% barium nitrate l mL again, shelters the SO that the template flag is introduced
4 2-To Ag
+Interference.Can add barium nitrate while with quantitative filter paper, burning shelters; The covering method of other interfering ion is seen appendix 1;
a
5. open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion and is advisable between 80%-100%, then with microsyringe, adds the 1.4mL sample solution to measure total chlorine ion concentration X in electrolytic cell
1
a
6. do blank test with above same method, record the concentration X of chlorion in blank
01
a
7. chloride content is calculated as follows:
In formula:
A Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g;
B. the mensuration of described content of inorganic chlorine:
b
1.Add sample consistent while with total chlorine, testing in the 100mL volumetric flask, accurately to 0.0001 g, recording its quality after weighing is m
2, water-soluble sample adds the distilled water constant volume, and the oil-soluble sample adds 95% ethanol constant volume, mixes;
b
2.By above-mentioned a
5Step is tested, and records inorganic chlorine ion concentration X in sample
2
b
3.With the salt content analyser, distilled water or 95% ethanol are carried out blank test, record chlorine ion concentration X in blank
02
b
4.Content of inorganic chlorine is calculated as follows:
In formula:
A Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g;
C. content of organic chloride %=
A Always-
A Nothing.
1.1 cut two onesize template flags by Fig. 1 requirement, one is used for blank, one is used for sample.Place the approximately absorbent cotton of 0.05 g in template flag central authorities that are used for sample, the paper using flag is rolled on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar, drip sample with 1 mL syringe on absorbent cotton, oil base sample sample weighting amount (0.05～0.10) g is advisable, water base sample sample weighting amount is advisable at (0.02～0.05) g, accurately to 0.0001 g, recording its quality is m
1, one is used for blank template flag and only places the approximately absorbent cotton of 0.05 g.Sample should be tried one's best consistent with blank absorbent cotton quality, the size of using.The medicament that volatility is low can replace the template flag with quantitative filter paper.
1.2 adding massfraction in the oxygen Molotov cocktail is each 2 mL of NaOH of 30% hydrogen peroxide and 0.1 mol/L.
1.3 with suitable flow velocity (liquid level is the microwaviness shape), pass into oxygen 2 min in the oxygen Molotov cocktail, then hold on the other hand the oxygen Molotov cocktail, another hand is picked up bottle stopper and light the template flag on spirit lamp, rapidly bottle stopper is carefully inserted bottleneck, build bottle stopper, withstand bottle stopper with hand and be inclined upwardly at the bottom of with the oxygen Molotov cocktail, make absorption liquid seal bottleneck.After all burnt was slightly cooling, jog oxygen Molotov cocktail several times, made the wetting bottle of absorption liquid wall, then placed 30 min to white cigarette disappearance.
1.4 rinse oxygen Molotov cocktail wall and steady arm three times with distillation moisture, then move in 100 mL volumetric flasks constant volume.If use the template flag, adding massfraction in absorption liquid is 0.2% barium nitrate l mL again, shelters the SO4 that the template flag is introduced
2-To Ag
+Interference.Can add barium nitrate while with quantitative filter paper, burning shelters.The covering method of other interfering ion is seen appendix 1.
1.5 open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion, and average conversion should be advisable between 80%-100%, adds 1.4 sample solutions of handling well to measure total chlorine ion concentration X with microsyringe in electrolytic cell afterwards
1.
1.6 do blank test with above same method, record the concentration X of chlorion in blank
01.
2, the mensuration of content of inorganic chlorine
2.1 add sample in 100 mL volumetric flasks, consistent when sample weighting amount is tested with total chlorine as far as possible, accurately to 0.0001 g, recording its quality after weighing is m
2, adding distilled water (the oil-soluble sample adds 95% ethanol), constant volume shakes up.
2.2 test by 1.5, record the concentration X of inorganic chlorine in sample
2.
2.3 with the salt content analyser, distilled water (95% ethanol) is carried out blank test, records the concentration X of chlorion in blank
02.
3, points for attention
3.1 during the mensuration of chloride content, if having black residue in oxygen Molotov cocktail absorption liquid, the interpret sample incomplete combustion, rekindle after should suitably reducing sample weighting amount.
3.2 each test all should be carried out blank test, the blank value substitution is calculated.Paper flag, degreasing Cottonopolis blank and that sample uses should be clean, and uniform quality, make blank value as far as possible little.
3.3 measured value is higher, measures after should suitably reducing sample weighting amount or corresponding dilute sample when the tack peak appears in instrument again.
3.4 repetition measurement standard specimen once again after working sample finishes, to determine accuracy and the stationarity of instrument.
4, result is calculated
4.1 chloride content calculates by formula (1)
In formula:
A
Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g.
4.2 content of inorganic chlorine calculates by formula (2)
In formula:
A
Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g.
4.3 content of organic chloride calculates by formula (3)
In formula:
A
Have---the content of organochlorine, %.
Appendix 1: the covering method of interfering ion
1.1 iodine and bromine
Beyond defluorination, in the time of titration chlorine, iodine and bromine will react with silver nitrate, interference measurement.Method for removing is in rare nitric acid medium, first uses oxygenant (as hydrogen peroxide) oxidation, then uses suitable solvent extraction.
1.2 oxygenant
In acid solution, Cr
2O
7 2-And ClO
3 -Deng can be Cl
-Be oxidized to Cl
2, interference measurement.Method for removing is that the pH that controls detected solution measured at 5～6 o'clock.
MnO
4 -With chlorine effect, interference measurement.Method for removing is to add lentamente appropriate 30%H
2O
2And 1mol/LHNO
3Mixed solution (1+10) in test solution, makes MnO
4 -Fade.
Oxygenant can silver oxide electrode, uses sodium sulphite, and ascorbic acid solution or other reductive agents that does not affect mensuration are processed and destroyed oxygenant.
1.3 nitrite
NO
2 -With Ag
+Generate AgNO
2Precipitation, interference measurement method for removing are to drip 10% sulfaminic acid solution in test solution, to without heating after Bubble formation, boiling.
1.4 sulfate
With Ag
+Generate the indissoluble sediment, interference measurement.Method for removing drips appropriate barium nitrate solution, generates barium sulphate, eliminates SO4
2-.
1.5 ammonium salt and iron (III) salt
While existing in a large number, mensuration is had interference, ammonium salt is to add 5% appropriate sodium carbonate liquor evaporate to dryness in 85 ℃ of water-baths, and NH rushes
3.Iron (III) salt is to add excessive sodium hydrate solution, boils, and removes by filter ferric hydroxide (III) precipitation of generation.A small amount of iron (III) the also way of available complex compound (as EDTA) is removed.
1.6 the ferricyanide and ferrocyanide
Add 2～3 times of zinc nitrates to sample size in test solution, be heated to boil, cooling.All move in volumetric flask, add water to scale, shake up, place layering,, with Filter Paper Dry filtration at a slow speed, discard initial filtrate, residual filtrate is for measuring.
Claims (1)
1. content of organic chloride method of testing in the oil recovery auxiliary agent is characterized in that this method of testing carries out as follows:
A. the mensuration of chloride content:
a
1.Cut two onesize template flags, at an absorbent cotton that is used for the placement 0.04-0.06g of template flag central authorities of sample, roll on the platinum filament that absorbent cotton is fixed on the Molotov cocktail support bar with the template flag, drip sample with the 1mL syringe on absorbent cotton, oil base sample sample weighting amount 0.05～0.10g, water base sample sample weighting amount is at 0.02～0.05g, and recording its quality is m
1Another is used for blank template flag and only places the consistent absorbent cotton of absorbent cotton that uses with sample;
a
2.Adding mass concentration in the oxygen Molotov cocktail is 28～32% hydrogen peroxide and each 2mL of NaOH of 0.08～0.12mol/L;
a
3.Pass into oxygen in the oxygen Molotov cocktail, time 1.5～2.5min, insert bottleneck with bottle stopper after then lighting the perfect combustion of template flag, will be inclined upwardly at the bottom of the oxygen Molotov cocktail, makes absorption liquid seal bottleneck; Jog oxygen Molotov cocktail after burning finishes, make the wetting bottle of absorption liquid wall, is placed to white cigarette and disappears;
a
4.Rinse oxygen Molotov cocktail wall and support bar three times with distillation moisture, then move to constant volume in the 100mL volumetric flask;
a
5. open the salt content analyzer, mix up bias voltage, add Cl after baseline is steady
-Standard specimen is measured average conversion at 80%-100%, then with microsyringe, adds the 1.4mL sample solution to measure total chlorine ion concentration X in electrolytic cell
1
a
6. do blank test with above same method, record the concentration X of chlorion in blank
01
a
7. chloride content is calculated as follows:
In formula:
A Always---chloride content, %;
X
1---the concentration of total chlorine in sample aqueous solution after burning, mg/L;
X
01---the concentration of chlorion in blank, mg/L;
m
l---sample mass, g;
B. the mensuration of content of inorganic chlorine:
b
1.Add sample consistent while with total chlorine, testing in the 100mL volumetric flask, recording its quality is m
2, water-soluble sample adds the distilled water constant volume, and the oil-soluble sample adds 95% ethanol constant volume, mixes;
b
2.By above-mentioned a
5Step is tested, and records inorganic chlorine ion concentration X in sample
2
b
3.With the salt content analyser, distilled water or 95% ethanol are carried out blank test, record chlorine ion concentration X in blank
02
b
4.Content of inorganic chlorine is calculated as follows:
In formula:
A Nothing---content of inorganic chlorine, %;
X
2---the concentration of inorganic chlorine in sample aqueous solution, mg/L;
X
02---the concentration of chlorion in blank, mg/L;
m
2---sample mass, g;
C. content of organic chloride %=
A Always-
A Nothing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210138619XA CN103389327A (en) | 2012-05-07 | 2012-05-07 | Method for testing organochlorine content of oil extraction auxiliary agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210138619XA CN103389327A (en) | 2012-05-07 | 2012-05-07 | Method for testing organochlorine content of oil extraction auxiliary agent |
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| Publication Number | Publication Date |
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Cited By (10)
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| CN103808556A (en) * | 2013-12-31 | 2014-05-21 | 上海新阳半导体材料股份有限公司 | Method for measuring total chlorine in methanesulfonic acid |
| CN105548320A (en) * | 2015-12-16 | 2016-05-04 | 广东石油化工学院 | Method for researching cracking of organic chlorine in crude oil |
| CN105717252A (en) * | 2016-03-11 | 2016-06-29 | 华电电力科学研究院 | Determination method for chlorine in coal |
| CN106556669A (en) * | 2015-09-25 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of method of content of organic chloride in measure Oilfield Chemicals |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN106840792A (en) * | 2017-01-04 | 2017-06-13 | 国家电网公司 | A kind of method of corrosivity chlorinity in detection fire-resistance oil |
| CN108717077A (en) * | 2018-03-20 | 2018-10-30 | 东营联合石化有限责任公司 | The detection method of crude oil content of organic chloride |
| CN109142350A (en) * | 2018-08-15 | 2019-01-04 | 山东阳谷华泰化工股份有限公司 | The detection method of chloride ion content in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts |
| CN110044762A (en) * | 2019-04-26 | 2019-07-23 | 华中科技大学 | A method of catalysis reduction-debromination measures total organic bromine content |
| CN112649527A (en) * | 2020-12-11 | 2021-04-13 | 广东省测试分析研究所（中国广州分析测试中心） | Method for measuring chlorine content in high-chlorine-content organic matter |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103808556A (en) * | 2013-12-31 | 2014-05-21 | 上海新阳半导体材料股份有限公司 | Method for measuring total chlorine in methanesulfonic acid |
| CN106556669A (en) * | 2015-09-25 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of method of content of organic chloride in measure Oilfield Chemicals |
| CN105548320A (en) * | 2015-12-16 | 2016-05-04 | 广东石油化工学院 | Method for researching cracking of organic chlorine in crude oil |
| CN105717252A (en) * | 2016-03-11 | 2016-06-29 | 华电电力科学研究院 | Determination method for chlorine in coal |
| CN106840792A (en) * | 2017-01-04 | 2017-06-13 | 国家电网公司 | A kind of method of corrosivity chlorinity in detection fire-resistance oil |
| CN106840792B (en) * | 2017-01-04 | 2019-06-28 | 国家电网公司 | A kind of method of corrosivity chlorinity in detection fire-resistance oil |
| CN106770408A (en) * | 2017-01-05 | 2017-05-31 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN106770408B (en) * | 2017-01-05 | 2019-09-27 | 国家电网公司 | The detection method of corrosivity chlorinity in a kind of fire-resistance oil |
| CN108717077A (en) * | 2018-03-20 | 2018-10-30 | 东营联合石化有限责任公司 | The detection method of crude oil content of organic chloride |
| CN109142350A (en) * | 2018-08-15 | 2019-01-04 | 山东阳谷华泰化工股份有限公司 | The detection method of chloride ion content in two hydration hexa-methylene -1,6- bisthiosulfate disodium salts |
| CN110044762A (en) * | 2019-04-26 | 2019-07-23 | 华中科技大学 | A method of catalysis reduction-debromination measures total organic bromine content |
| CN112649527A (en) * | 2020-12-11 | 2021-04-13 | 广东省测试分析研究所（中国广州分析测试中心） | Method for measuring chlorine content in high-chlorine-content organic matter |
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