CN104458602A - Rapid determination method for high mineralization degree oilfield sewage suspended matters - Google Patents

Rapid determination method for high mineralization degree oilfield sewage suspended matters Download PDF

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CN104458602A
CN104458602A CN201310416413.3A CN201310416413A CN104458602A CN 104458602 A CN104458602 A CN 104458602A CN 201310416413 A CN201310416413 A CN 201310416413A CN 104458602 A CN104458602 A CN 104458602A
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absorbance
sample
sewage
sodium chloride
chloride solution
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CN104458602B (en
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陆伟
单全生
宋中华
陈广明
何新兴
谭川江
伍轶鸣
王振波
吕志凤
陈文�
刘生勇
郑伟涛
林清金
张丽
蒋宏
张晓哲
王吉福
柳楠
夏晓晖
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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Abstract

Belonging to the technical field of oilfield sewage suspended matter determination, the invention provides a rapid determination method for high mineralization degree oilfield sewage suspended matters. The method includes: taking a sewage sample airtightly according to provisions; dividing the sewage sample into two parts, diluting one part of the sewage sample with a sodium chloride solution according to different proportions, taking a dilution sodium chloride solution to conduct blank correction, and measuring the absorbance of diluted sewage sample respectively; measuring the content of suspended matters in the other part of sewage sample by a gravimetric method; correlating the gravimetric method measurement result with the absorbance, determining the content of suspended matters under each absorbance through the proportional relation, and establishing an absorbance-suspended matter content standard curve; and injecting the to-be-determined sewage sample into a cuvette. The method provided by the invention has the characteristics of easy operation, low cost, short time and high accuracy, by directly using water sample itself as the reference substance, using brine with equal mineralization degree to sewage to treat the water sample by dilution, and combining the gravimetric method to draw the standard curve, the interference of salt, floating oil and dissolved oil in the water sample to absorbance can be avoided.

Description

A kind of High Mineralized Oilfield Wastewater suspension rapid assay methods
Technical field
The present invention relates to a kind of High Mineralized Oilfield Wastewater suspension rapid assay methods, belong to oilfield sewage suspended matter determination technical field.
Background technology
After disposing polluted water in oil, re-injection not only can effectively utilize water source to carry out oil extraction, is also the important measures of Conservation areas water body environment simultaneously.Suspension is one of important monitoring index of return water, and carrying out Real-Time Monitoring exactly to it is the major issue that each oil field can not be ignored.But, it is large that membrane filter technique (also weigh method) in the petroleum industry standard " petroclastic rock reservoir water fertilizer index and analytical approach " that current oil field generally performs has error, cost is high, many drawbacks such as length consuming time, especially for High Mineralized Oilfield Wastewater, cyclic washing filter membrane after filtration, is needed, complex operation, consuming time, if containing ferrous iron in sewage, then in filtration, washing process, ferrous oxidation often causes result higher.Utilize optical means to carry out suspension content and measure the key breakthrough mouth more and more becoming and find on-line monitoring.In some reports, have scholar with the suspension reference material drawing standard curve of zeyssatite as simulation, this is infeasible in oily water treatment.Oil slick in oily sewage and dissolved oil also have the extinction of some strength under certain wavelength, disturb to suspended matter determination.Above problem is there is equally in the white high molecular polymer that the spectrophotometric method hydrazine sulfate mentioned in GB " mensuration of GB/13200-1911 water turbidity " and hexamethylenetetramine polymerization are formed as reference material, and hydrazine sulfate is extremely toxic substance, has carcinogenesis.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of High Mineralized Oilfield Wastewater suspension rapid assay methods.
A kind of High Mineralized Oilfield Wastewater suspension rapid assay methods, comprises the steps:
Step a. is airtight according to the rules gets sewage sample;
Got sewage sample is divided into two parts by step b., wherein will make blank correction by after different proportion dilution with dilution sodium chloride solution by a part of sewage sample sodium chloride solution, and survey the absorbance of the rear sewage sample of dilution respectively; By another part sewage sample gravimetric determination suspension content;
Gravimetric determination result associates with absorbance by step c, and passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve;
Steps d. Wastewater Sample to be measured is injected cuvette, under the wavelength that step b is used, measures the absorbance of sewage to be measured;
Step e. finds the suspension content corresponding to this absorbance from the typical curve of step c gained.
As preferably, the mass percent concentration of the dilution sodium chloride solution adopted in described step b is 10% ~ 20%.
As preferably, the concentration of described dilution sodium chloride solution is consistent with the total mineralization of Wastewater Sample.
As preferably, in described step b, sewage sample is poured in several 50ml color comparison tubes respectively according to certain volume gradient, and is diluted to scale with sodium chloride solution, thus obtain the sewage sample of different dilution ratio.
As preferably, first sewage was rocked evenly before mensuration sewage absorbance.
As preferably, in described step a, during sampling, adopt the polyethylene bottle enclosed sampling of tool plug, prevent the mensuration affecting absorbance because quick-fried oxygen produces Fe forms.
As preferably, when the absorbance of the Wastewater Sample of described steps d gained exceeds standard curve range, survey absorbance again after diluting with the sodium chloride solution identical with the concentration of sodium chloride solution that step b adopts, measured result is multiplied by corresponding extension rate can draw former water sample suspension content.
Compared with prior art, beneficial effect of the present invention is:
Method of the present invention is easy to operate, cost is low, consuming time short, accuracy is higher, by directly adopting water sample itself as primary standard substance, with the salt solution dilution process process water sample with salinities such as sewage, in conjunction with gravimetric method drawing standard curve, avoid the interference that the salinity in water sample, oil slick and dissolved oil produce absorbance.The present invention is especially applicable to the water quality Real-Time Monitoring of hay tank water outlet to well head.
Embodiment
Obviously, the many modifications and variations that those skilled in the art do based on aim of the present invention belong to protection scope of the present invention.
A kind of High Mineralized Oilfield Wastewater suspension, comprises the steps: that a. is airtight according to the rules and gets sewage sample; B. got sewage sample is divided into two parts, wherein will makes blank correction by after different proportion dilution with dilution sodium chloride solution by a part of sewage sample sodium chloride solution, and survey the absorbance of the rear sewage sample of dilution respectively; By another part sewage sample gravimetric determination suspension content; C. gravimetric determination result associated with absorbance, passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve; D. Wastewater Sample to be measured is injected cuvette, under the wavelength that step b is used, measure the absorbance of sewage to be measured; E. the suspension content corresponding to this absorbance is found from the typical curve of step c gained.The inventive method can Fast Measurement wastewater suspended substance content.
High Mineralized Oilfield Wastewater suspension, comprises the steps:
Step a. is airtight according to the rules gets sewage sample;
Got sewage sample is divided into two parts by step b., wherein will make blank correction by after different proportion dilution with dilution sodium chloride solution by a part of sewage sample sodium chloride solution, and survey the absorbance of the rear sewage sample of dilution respectively; By another part sewage sample gravimetric determination suspension content;
Gravimetric determination result associates with absorbance by step c, and passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve;
Steps d. Wastewater Sample to be measured is injected cuvette, under the wavelength that step b is used, measures the absorbance of sewage to be measured;
Step e. finds the suspension content corresponding to this absorbance from the typical curve of step c gained.
The mass percent concentration of the dilution sodium chloride solution adopted in described step b is 10% ~ 20%.
The concentration of described dilution sodium chloride solution is consistent with the total mineralization of Wastewater Sample.
In described step b, sewage sample is poured in several 50ml color comparison tubes respectively according to certain volume gradient, and is diluted to scale with sodium chloride solution, thus obtain the sewage sample of different dilution ratio.
First sewage was rocked evenly before mensuration sewage absorbance.
In described step a, during sampling, adopt the polyethylene bottle enclosed sampling of tool plug, prevent the mensuration affecting absorbance because quick-fried oxygen produces Fe forms.
When the absorbance of the Wastewater Sample of described steps d gained exceeds standard curve range, survey absorbance again after diluting with the sodium chloride solution identical with the concentration of sodium chloride solution that step b adopts, measured result is multiplied by corresponding extension rate can draw former water sample suspension content.
According to Lambert-Beer's law, can extinction material absorbance under visible light and its concentration linear, accordingly, by drawing the suspension content in concentration of suspension-absorbance standard curve Fast Measurement sewage sample.
High Mineralized Oilfield Wastewater suspension, comprises the steps:
Step (1), according to rower regulation enclosed sampling, the polyethylene bottle of apparatus plug was learnt from else's experience the water sample after breakdown of emulsion, coagulation, sedimentation; Prevent the Fe forms produced because of quick-fried oxygen from causing water colour to deepen and affecting the mensuration of absorbance;
Step (2), got sewage sample is divided into two parts processes, part sewage sample is poured in several 50ml color comparison tubes according to certain volume gradient after fully shaking and shaking up respectively, and be diluted to scale with the sodium chloride solution of 10 ~ 20%, thus obtain the sewage sample of different dilution ratio; The concentration of dilution sodium chloride solution is consistent with the total mineralization of Wastewater Sample.Measurement result can be made more accurate.
Step (3), spectrophotometer wavelength is adjusted to suitable wavelength, the wavelength that the present embodiment adopts is 420nm, does blank correction with the dilution sodium chloride solution in step (2);
Step (4), use 1cm cuvette, adopt 420nm wavelength to measure the absorbance of sewage sample in each color comparison tube respectively, before mensuration, need color comparison tube shaking to make distribution of particles even as far as possible for several times;
Step (5), by another part sewage sample according to the suspended matter determination standard method performed in " petroclastic rock reservoir water fertilizer index and analytical approach " and gravimetric determination suspension content;
Step (6), measurement result associated with absorbance, passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve;
Step (7), the Wastewater Sample to be measured sampling spot each in slave station or well head fetched inject cuvette, measure its absorbance under the wavelength used when drawing standard curve;
Step (8), find the suspension content corresponding to this absorbance from typical curve.
Preferred as above-described embodiment, when the absorbance of the Wastewater Sample of described step (7) gained exceeds standard curve range, survey absorbance again after diluting with the sodium chloride solution identical with the concentration of sodium chloride solution that step (2) adopts, measured result is multiplied by corresponding extension rate can draw former water sample suspension content.
It should be understood that to those skilled in the art and wavelength the sensitiveest should be adopted to improve the accuracy of measurement result for different liquid.The wavelength of 420nm is adopted in the present embodiment.
Following table 1 is the measurement result to certain oil-contaminated water of oil field, as shown in table 1.
Table 1
Sample tap Gravimetric method (mg/L) The present invention (mg/L) Relative deviation/%
Slurry tank exports 14.50 14.38 0.83
One-level filter tank exports 3.25 3.22 0.92
Secondary filter tank exports 2.40 2.44 1.67
Certain well head 2.80 2.89 3.21
The gravimetric method relative deviation basic controlling of this method and standard is shown below 5% by table 1.
Above embodiment is only exemplary embodiment of the present invention, and be not used in restriction the present invention, protection scope of the present invention is defined by the claims.Those skilled in the art can in essence of the present invention and protection domain, and make various amendment or equivalent replacement to the present invention, this amendment or equivalent replacement also should be considered as dropping in protection scope of the present invention.

Claims (6)

1. a High Mineralized Oilfield Wastewater suspension rapid assay methods, is characterized in that comprising the steps:
Step a. is airtight according to the rules gets sewage sample;
Got sewage sample is divided into two parts by step b., wherein will make blank correction by after different proportion dilution with dilution sodium chloride solution by a part of sewage sample sodium chloride solution, and survey the absorbance of the rear sewage sample of dilution respectively; By another part sewage sample gravimetric determination suspension content;
Gravimetric determination result associates with absorbance by step c, and passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve;
Steps d. Wastewater Sample to be measured is injected cuvette, under the wavelength that step b is used, measures the absorbance of sewage to be measured;
Step e. finds the suspension content corresponding to this absorbance from the typical curve of step c gained.
2. High Mineralized Oilfield Wastewater suspension rapid assay methods according to claim 1, is characterized in that the mass percent concentration of the dilution sodium chloride solution adopted in described step b is 10% ~ 20%;
The concentration of described dilution sodium chloride solution is consistent with the total mineralization of Wastewater Sample.
3. High Mineralized Oilfield Wastewater suspension rapid assay methods according to claim 1; it is characterized in that in described step b; sewage sample is poured in several 50ml color comparison tubes according to certain volume gradient respectively; and be diluted to scale with sodium chloride solution, thus obtain the sewage sample of different dilution ratio; First sewage was rocked evenly before mensuration sewage absorbance.
4. High Mineralized Oilfield Wastewater suspension rapid assay methods according to claim 1, is characterized in that in described step a, adopts the polyethylene bottle enclosed sampling of tool plug during sampling, prevents the mensuration affecting absorbance because quick-fried oxygen produces Fe forms.
5. High Mineralized Oilfield Wastewater suspension rapid assay methods according to claim 1, when it is characterized in that the absorbance of the Wastewater Sample of described steps d gained exceeds standard curve range, survey absorbance again after diluting with the sodium chloride solution identical with the concentration of sodium chloride solution that step b adopts, measured result is multiplied by corresponding extension rate can draw former water sample suspension content.
6. High Mineralized Oilfield Wastewater suspension rapid assay methods according to claim 1, is characterized in that:
Step (1), according to rower regulation enclosed sampling, the polyethylene bottle of apparatus plug was learnt from else's experience the water sample after breakdown of emulsion, coagulation, sedimentation; Prevent the Fe forms produced because of quick-fried oxygen from causing water colour to deepen and affecting the mensuration of absorbance;
Step (2), got sewage sample is divided into two parts processes, part sewage sample is poured in several 50ml color comparison tubes according to certain volume gradient after fully shaking and shaking up respectively, and be diluted to scale with the sodium chloride solution of 10 ~ 20%, thus obtain the sewage sample of different dilution ratio; The concentration of dilution sodium chloride solution is consistent with the total mineralization of Wastewater Sample;
Step (3), spectrophotometer wavelength is adjusted to suitable wavelength, the wavelength that the present embodiment adopts is 420nm, does blank correction with the dilution sodium chloride solution in step (2);
Step (4), use 1cm cuvette, adopt 420nm wavelength to measure the absorbance of sewage sample in each color comparison tube respectively, before mensuration, need color comparison tube shaking to make distribution of particles even as far as possible for several times;
Step (5), by another part sewage sample according to the suspended matter determination standard method performed in " petroclastic rock reservoir water fertilizer index and analytical approach " and gravimetric determination suspension content;
Step (6), measurement result associated with absorbance, passing ratio relation determines each absorbance low suspension thing content, sets up absorbance-suspension content typical curve;
Step (7), the Wastewater Sample to be measured sampling spot each in slave station or well head fetched inject cuvette, measure its absorbance under the wavelength used when drawing standard curve;
Step (8), find the suspension content corresponding to this absorbance from typical curve;
When the absorbance of the Wastewater Sample of described step (7) gained exceeds standard curve range, survey absorbance again after diluting with the sodium chloride solution identical with the concentration of sodium chloride solution that step (2) adopts, measured result is multiplied by corresponding extension rate can draw former water sample suspension content.
CN201310416413.3A 2013-09-13 2013-09-13 A kind of High Mineralized Oilfield Wastewater suspension rapid assay methods Active CN104458602B (en)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN108801745A (en) * 2017-05-02 2018-11-13 中国石油天然气股份有限公司 A kind of suspended solids content test device
CN113092304A (en) * 2021-03-31 2021-07-09 神华神东煤炭集团有限责任公司 Method for detecting content of coal in gear oil of coal mine in-use equipment

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CN101551319A (en) * 2009-05-05 2009-10-07 天津大学 Method for measuring concentration of suspended particles in the drainage of sewage treatment industry
CN102001739A (en) * 2010-09-29 2011-04-06 鄯善华油技术服务有限公司 Water quality standard technology for treating oily sewage
CN102608053A (en) * 2012-02-23 2012-07-25 北京水泥厂有限责任公司 Detection method for mineral oil in sludge

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108801745A (en) * 2017-05-02 2018-11-13 中国石油天然气股份有限公司 A kind of suspended solids content test device
CN113092304A (en) * 2021-03-31 2021-07-09 神华神东煤炭集团有限责任公司 Method for detecting content of coal in gear oil of coal mine in-use equipment

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