CN101825579A - Method for measuring concentration of polyacrylamide solution - Google Patents
Method for measuring concentration of polyacrylamide solution Download PDFInfo
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- CN101825579A CN101825579A CN201010178354A CN201010178354A CN101825579A CN 101825579 A CN101825579 A CN 101825579A CN 201010178354 A CN201010178354 A CN 201010178354A CN 201010178354 A CN201010178354 A CN 201010178354A CN 101825579 A CN101825579 A CN 101825579A
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Abstract
The invention relates to a method for measuring concentration of partial hydrolyzed polyacrylamide in oilfield extraction solution. Reagents used by the method have no toxicity, low requirement for experiment condition, simple and convenient operation and good repeatability. The invention adopts the technical scheme that the method comprises the following steps: measuring a series of colloid titration values by adopting a colloid titration method, establishing a standard curve of the colloid titration values V and the corresponding concentration C, and fitting a calculation formula; adding excessive standard positive ion reagent PD into the partial hydrolyzed polyacrylamide solution with the concentration to be measured, titrating the excessive standard positive ion reagent by adopting standard solution of negative ion reagent PVSK, and measuring the colloid titration value required at a titration end point by using TBO as an indicator; and performing three groups of parallel experiments on a sample to be tested and taking a mean value, substituting the mean value into the fitted calculation formula, and solving the concentration of the polyacrylamide. The method has high measurement precision and accuracy, provides a convenient and feasible detection method for an oilfield, and can be used for measuring the concentration of the partial hydrolyzed polyacrylamide in the oilfield extraction solution.
Description
Technical field
The present invention relates to a kind of assay method of concentration of polyacrylamide solution, belong to the quantitative test field.Be particularly suitable for the mensuration of partially hydrolyzed polyacrylamide in the oil field mining liquid (HPAM) concentration.
Background technology
HPAM is the present synthesizing water-solubility high polymer chemistry product of turnout maximum in the world, is widely used in many production divisions such as improving oil recovery, drilling well, ore dressing, papermaking, medicine, water treatment.The concentration of analyzing injection, extraction liquid polymkeric substance quickly and accurately is one of main contents of production run dynamic monitoring, is the important means that guarantees to produce normal operation.Whether concentration analysis accurately influences the design of field test scheme and industrialization injecting scheme.Therefore, how quick, accurately the concentration of polymkeric substance is significant in the quantitative measurement oil field mining liquid.
At present, the method for measurement of concentration of polymkeric substance (HPAM) mainly contains gel permeation chromatography, starch-cadmium iodide method, nephelometry and viscosimetry in the extraction liquid.Since the complicacy of field use situation and condition, the gel permeation chromatography complex operation, required instrument is more and expensive, and operating conditions is difficult in the production scene satisfy.The universality and the reappearance of starch-cadmium iodide method and these two kinds of methods of nephelometry are also relatively poor, but also have used bromine water and the glacial acetic acid that is easy to volatilize, and the healthy of testing staff is harmful to.Though and viscosimetry is easy fast, accuracy and degree of accuracy that high salinity industrial waste waters such as oil field are measured all are difficult to reach requirement.Therefore, the detection accuracy of polymer concentration can't be determined so far in the extraction liquid.
Summary of the invention
The objective of the invention is: the assay method of the concentration of polyacrylamide that in order to overcome the deficiency of existing analytical technology, the spy provides that a kind of agents useful for same is nontoxic, environmentally safe,, favorable reproducibility low, simple and efficient to handle to requirement for experiment condition, measuring accuracy and accuracy are high.
The colloid titration method that uses among the present invention is based between positive and negative ion because electrostatic interaction forms charge ratio is the principle of 1: 1 poly ion complexes, makes titer carries out electric charge mensuration to sample to be tested a kind of method with the polyelectrolyte of known charge density.For positive colloid (cationic polyelectrolyte) is to be titration reagent with negative colloid (anionic polyelectrolyte) standard solution PVSK (polyvinyl sulfuric acid potassium); For negative colloid then is to add excessive standard positive ion reagent PD (diallyl dimethyl ammoniumchloride) and then with the positive ion reagent of PVSK titration surplus.Judge terminal point with color indicator blutene (TBO).Do not react and present blue greenly at first because the TBO indicator has positive charge and cationic polyelectrolyte, indicator and PVSK react the generation heterochromaty after negative colloid PVSK and cationic polyelectrolyte reaction end when titration.Sample solution becomes aubergine immediately.
The present invention solves this technical matters by the following technical solutions:
A kind of assay method of concentration of polyacrylamide solution, it is characterized in that: for the method for measurement of concentration of anion-polyacrylamide solution, comprise following three steps: step 1, get the PDDA code name PD standard solution of 3mL0.01% earlier and put into the 50mL triangular flask, drip a blutene code name TBO indicator again, use 0.01% polyvinyl sulfuric acid potassium code name PVSK standard solution titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
0Step 2, get the polymer solution of 0.1～3mL series concentration and put into the 50mL triangular flask respectively, regulating liquid to be measured to pH value with NaOH or hydrochloric acid is 9～10, the PD standard solution that adds 3mL0.01% again stirred 10 minutes, drip a TBO indicator, use 0.01% PVSK titer titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
1, obtain colloid drops definite value (V
0-V
1), set up (V with a series of colloid drops definite values that obtain with corresponding concentration C
0-V
1)-C typical curve, and simulate computing formula V between colloid drops definite value and the concentration
0-V
1=nC+n
1Step 3 is carried out titration operation according to step 1,2 pairs of samples to be tested, does three groups of parallel laboratory tests and averages, and obtains the colloid drops definite value; With the computing formula that step 3 resulting colloid drops definite value substitution step 2 is simulated, calculate the concentration of polyacrylamide in the sample to be tested.
For the cationic-type polyacrylamide Measurement Of The Concentration Of Solution, comprise following two steps, step 1, get the polymer solution of 0.1～3mL series concentration earlier and put into the 50mL triangular flask respectively, regulate pH value to 2～3 of liquid to be measured with NaOH or hydrochloric acid, drip a TBO indicator, use 0.01% PVSK titer titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
0, do the volume that a blank test consumes the PVSK standard solution according to abovementioned steps 1 and be designated as V
1, with a series of colloid drops definite value (V that obtain
0-V
1) set up (V with corresponding concentration C
0-V
1)-C typical curve, and simulate computing formula between colloid drops definite value and the concentration; Step 2 is carried out titration operation according to 1 pair of sample to be tested of above-mentioned steps, does three groups of parallel laboratory tests and averages, and obtains the colloid drops definite value; The computing formula that step 2 resulting colloid drops definite value substitution step 1 is simulated at last calculates the concentration of polyacrylamide in the sample to be tested.
For described series concentration is respectively 5,10,20,30,40,50,60,70,80,90,100,110,120,130,140 or this kind polymkeric substance standard solution of 150mg/L; Set up typical curve with the serial colloid drops definite value and the corresponding concentration that obtain, need this kind polymkeric substance standard solution to be at least 5 parts.
Computing formula V for colloid drops definite value and concentration
0-V
1=nC+n
1, constant n, n
1Be respectively the slope and the intercept of colloid drops definite value～concentration standard curve.
The medicine and the instrument that need among the present invention to use are:
A, medicine: PDDA (PD), polyvinyl sulfuric acid potassium (PVSK), blutene indicator (TBO), 0.5% NaOH or hydrochloric acid.
B, instrument: microburette, transfer pipet, volumetric flask, conical flask, magnetic stirrer, pH meter.
Agents useful for same compound method of the present invention is:
The preparation of a, 0.01%PVSK standard solution
Take by weighing polyvinyl sulfuric acid potassium (PVSK) 0.0500g, be dissolved in the 500mL volumetric flask, be diluted to scale with deionized water.Obtain 0.01% PVSK standard solution.
The preparation of b, 0.01%PD standard solution
Accurately absorption concentration is poly dimethyl dipropenyl ammonium chloride stoste 1mL constant volume in the 100mL volumetric flask of 20%, and obtaining concentration is the PD solution of 2000ppm; Accurately draw PD solution constant volume in the 100mL volumetric flask of this 2000ppm of 5mL, obtain 0.01% PD standard solution.
The preparation of c, 0.1%TBO indicator solution
In 100mL distilled water, be stored in the brown indicator dropper bottle standby 0.10g blutene powder dissolution.
The configuration of d, polymkeric substance (1000mg/L) storing solution
In the 50mL beaker, add about 30mL distilled water (or preparation clear water), accurately take by weighing the 0.1000g polymeric aggregate, be sprinkled in the beaker equably and place, all be transferred in the 100mL volumetric flask after the swelling, repeatedly wash beaker, also transfer to the water that washed in the volumetric flask, shaking volumetric flask makes bottle interior solution even, in volumetric flask, add water to scale, shake up solution, as the polymkeric substance storing solution.
The present invention compared with the prior art, have following beneficial effect: (1) method of the present invention not only is fit to the mensuration of cationic-type polyacrylamide concentration, also being fit to anion-polyacrylamide is the mensuration of partially hydrolyzed polyacrylamide concentration, is particularly suitable under oil field salinity height, the high environment of calcium ions and magnesium ions content the mensuration of partially hydrolyzed polyacrylamide concentration in the extraction liquid; (2) nontoxic, the environmentally safe of this assay method agents useful for same,, favorable reproducibility low, simple and efficient to handle to requirement for experiment condition; (3) this method measuring accuracy and accuracy height for field test mechanism in oil field provides the detection method of the feasible and science of a kind of convenience, can be used for the mensuration of concentration of polyacrylamide in the oil field mining liquid.
Description of drawings
Fig. 1 is the canonical plotting of embodiment 1.
Fig. 2 is the canonical plotting of embodiment 2.
Fig. 3 is the canonical plotting of embodiment 3.
Among the figure: horizontal ordinate, concentration C, the ppm of unit; Ordinate, colloid drops definite value V, Unit.
Embodiment
The invention will be further described below in conjunction with concrete drawings and Examples.
The mensuration that degree of hydrolysis is 35%, molecular weight is 1,200 ten thousand concentration of polyacrylamide solution
A, this kind polymkeric substance storing solution (1000mg/L) is diluted to concentration with simulation salt solution is respectively 5,10,20,30,40,50,60,70,80,90,100,110,120,130,140 and the standard solution of 150mg/L.
B, the PDDA code name PD standard solution of getting 3mL0.01% are earlier put into the 50mL triangular flask, drip a blutene code name TBO indicator again, use 0.01% polyvinyl sulfuric acid potassium code name PVSK standard solution titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
0
C, the polymer solution of getting series concentration among the 3mL a are put into the 50mL triangular flask respectively, regulating liquid to be measured pH value extremely with NaOH or hydrochloric acid is 9～10, the PD standard solution that adds 3mL0.01% again stirred 10 minutes, drip a TBO indicator, use 0.01% PVSK titer titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
1, obtain colloid drops definite value (V
0-V
1).
D, the serial colloid drops definite value (V that will obtain
0-V
1) utilize mapping software to set up (V with corresponding concentration
0-V
1)-C typical curve (Fig. 1), and the expression formula that simulates colloid drops definite value and concentration C is: V
0-V
1=0.012C+0.0201.
Table 1
| Colloid drops definite value mL | Actual concentrations mg/L | Calculating concentration mg/L | Relative error % |
| ??0.14 | ??10 | ??10.0 | ??0 |
| ??0.39 | ??30 | ??30.8 | ??2.7 |
| ??0.62 | ??50 | ??50.0 | ??0 |
| ??0.89 | ??70 | ??72.5 | ??2.5 |
| Colloid drops definite value mL | Actual concentrations mg/L | Calculating concentration mg/L | Relative error % |
| ??1.20 | ??100 | ??98.3 | ??1.7 |
| ??1.48 | ??120 | ??121.7 | ??1.4 |
| ??1.69 | ??140 | ??139.2 | ??0.6 |
E, be 10,30,50,70,100,120 and resulting colloid drops definite value substitution expression formula " V during 140mg/L with concentration
0-V
1=0.012C+0.0201 " in, corresponding calculating concentration obtained.The calculating concentration and the actual concentrations that obtain are contrasted to verify the rationality of this expression formula, and result's contrast sees Table 1.
From table 1 the comparative illustration match of calculating concentration and actual concentrations very near actual conditions, show that test result of the present invention has good accuracy.
The mensuration that degree of hydrolysis is 42%, molecular weight is 1,200 ten thousand concentration of polyacrylamide solution
A, polymkeric substance storing solution (1000mg/L) is diluted to concentration with simulation salt solution is respectively 5,10,20,30,40,50,60,70,80,90,100,110,120,130,140 and the standard solution of 150mg/L.
Operation steps b, c in b, the repetition example 1
C, the serial colloid drops definite value (V that will obtain
0-V
1) utilize mapping software to set up (V with corresponding concentration
0-V
1)-C typical curve (Fig. 2), and the expression formula that simulates colloid drops definite value and concentration C is: V
0-V
1=0.0167C+0.0157.
D, be 10,30,50,70,100,120 and resulting colloid drops definite value substitution expression formula " V during 140mg/L with concentration
0-V
1=0.0167C+0.0157 " in, corresponding calculating concentration obtained.The calculating concentration and the actual concentrations that obtain are contrasted to verify the rationality of this expression formula, and result's contrast sees Table 2.
Table 2
| Colloid drops definite value mL | Actual concentrations mg/L | Calculating concentration mg/L | Relative error % |
| ??0.19 | ??10 | ??10.4 | ??4.0 |
| ??0.34 | ??20 | ??19.4 | ??3.0 |
| ??0.66 | ??40 | ??38.6 | ??3.5 |
| ??1.05 | ??60 | ??61.9 | ??3.2 |
| ??1.49 | ??90 | ??88.3 | ??1.9 |
| ??1.90 | ??110 | ??112.8 | ??2.5 |
| ??2.18 | ??130 | ??129.6 | ??0.3 |
From table 2 the comparative illustration match of calculating concentration and actual concentrations very near actual conditions, show that test result of the present invention has good accuracy.
The mensuration that degree of hydrolysis is 45%, molecular weight is 1,200 ten thousand concentration of polyacrylamide solution
A, polymkeric substance storing solution (1000mg/L) is diluted to concentration with simulation salt solution is respectively 5,10,20,30,40,50,60,70,80,90,100,110,120,130,140 and the standard solution of 150mg/L.
Operation steps b, c in b, the repetition example 1
C, the serial colloid drops definite value (V that will obtain
0-V
1) utilize mapping software to set up (V with corresponding concentration
0-V
1)-C typical curve (Fig. 3), and the expression formula that simulates colloid drops definite value and concentration C is: V
0-V
1=0.0179C+0.0435.
D, be 10,30,50,70,100,120 and resulting colloid drops definite value substitution expression formula " V during 140mg/L with concentration
0-V
1=0.0179C+0.0435 " in, corresponding calculating concentration obtained.The calculating concentration and the actual concentrations that obtain are contrasted to verify the rationality of this expression formula, and result's contrast sees Table 3.
Table 3
| Colloid drops definite value mL | Actual concentrations mg/L | Calculating concentration mg/L | Relative error % |
| ??0.22 | ??10 | ??9.9 | ??1.0 |
| ??0.59 | ??30 | ??30.5 | ??1.7 |
| ??0.95 | ??50 | ??50.6 | ??1.2 |
| ??1.35 | ??70 | ??73.0 | ??4.3 |
| ??1.80 | ??100 | ??98.1 | ??1.9 |
| ??2.21 | ??120 | ??121.0 | ??0.8 |
| ??2.55 | ??140 | ??140.0 | ??0 |
From table 3 the comparative illustration match of calculating concentration and actual concentrations very near actual conditions, show that test result of the present invention has good accuracy.
From above three groups of experimental datas as can be seen, relative error of the present invention all in 5%, meets the accuracy requirement of titration experiments.In addition, the inventive method agents useful for same is nontoxic, environmentally safe,, favorable reproducibility low, simple and efficient to handle to requirement for experiment condition, measuring accuracy and accuracy height, and the detection method of the feasible and science of convenience is provided for field test mechanism.
Claims (4)
1. the assay method of a concentration of polyacrylamide solution, it is characterized in that: for the anion-polyacrylamide Measurement Of The Concentration Of Solution, comprise following three steps: step 1, get the PDDA code name PD standard solution of 3mL0.01% earlier and put into the 50mL triangular flask, drip a blutene code name TBO indicator again, use 0.01% polyvinyl sulfuric acid potassium code name PVSK standard solution titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
0Step 2, get the polymer solution of 0.1～3mL series concentration and put into the 50mL triangular flask respectively, regulating liquid to be measured to pH value with NaOH or hydrochloric acid is 9～10, the PD standard solution that adds 3mL0.01% again stirred 10 minutes, drip a TBO indicator, use 0.01% PVSK titer titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
1, obtain colloid drops definite value (V
0-V
1), set up (V with a series of colloid drops definite values that obtain with corresponding concentration C
0-V
1)-C typical curve, and simulate computing formula V between colloid drops definite value and the concentration
0-V
1=nC+n
1Step 3 is carried out titration operation according to step 1,2 pairs of samples to be tested, does three groups of parallel laboratory tests and averages, and obtains the colloid drops definite value; With the computing formula that step 3 resulting colloid drops definite value substitution step 2 is simulated, calculate the concentration of polyacrylamide in the sample to be tested.
2. assay method of concentration of polyacrylamide solution according to claim 1, it is characterized in that: for the cationic-type polyacrylamide Measurement Of The Concentration Of Solution, comprise following two steps, step 1, get the polymer solution of 0.1～3mL series concentration earlier and put into the 50mL triangular flask respectively, regulate pH value to 2～3 of liquid to be measured with NaOH or hydrochloric acid, drip a TBO indicator, use 0.01% PVSK titer titration to the aubergine terminal point then, the volume of used PVSK standard solution is designated as V
0, do the volume that a blank test consumes the PVSK standard solution according to abovementioned steps 1 and be designated as V
1, with a series of colloid drops definite value (V that obtain
0-V
1) set up (V with corresponding concentration C
0-V
1)-C typical curve, and simulate computing formula between colloid drops definite value and the concentration; Step 2 is carried out titration operation according to 1 pair of sample to be tested of above-mentioned steps, does three groups of parallel laboratory tests and averages, and obtains the colloid drops definite value; The computing formula that step 2 resulting colloid drops definite value substitution step 1 is simulated at last calculates the concentration of polyacrylamide in the sample to be tested.
3. according to the assay method of claim 1 or 2 described concentration of polyacrylamide solution, it is characterized in that: described series concentration is 5,10,20,30,40,50,60,70,80,90,100,110,120,130,140 or this kind polymkeric substance standard solution of 150mg/L; Set up typical curve with the serial colloid drops definite value and the corresponding concentration that obtain, need this kind polymkeric substance standard solution to be at least 5 parts.
4. according to the assay method of claim 1 or 2 described concentration of polyacrylamide solution, it is characterized in that: the computing formula V of colloid drops definite value and concentration
0-V
1=nC+n
1, constant n, n
1Be respectively the slope and the intercept of colloid drops definite value～concentration standard curve.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588809A (en) * | 2015-12-15 | 2016-05-18 | 新疆科力新技术发展股份有限公司 | Method for measuring concentration of polyacrylamide in oil field polymer-flooding produced liquid |
| CN107941985A (en) * | 2018-01-12 | 2018-04-20 | 中国海洋石油集团有限公司 | A kind of partially hydrolyzed polyacrylamide (PHPA) suitable for offshore oilfield is birdsed of the same feather flock together the detection method of compound concentration |
| CN108548891A (en) * | 2018-03-13 | 2018-09-18 | 大丰跃龙化学有限公司 | A kind of analysis method detecting polyhexamethylene list guanidine using mixed indicator |
| CN111272612A (en) * | 2020-03-03 | 2020-06-12 | 西南石油大学 | Primary screening method of demulsifier |
| CN111595963A (en) * | 2020-04-30 | 2020-08-28 | 中国石油天然气股份有限公司 | Method for measuring hydrolysis degree of partially hydrolyzed polyacrylamide in oil-gas field chemical flooding output fluid |
| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
| CN112986052A (en) * | 2019-12-13 | 2021-06-18 | 中国石油天然气股份有限公司 | Method for testing concentration of polyacrylamide and application thereof |
| CN114441661A (en) * | 2020-11-03 | 2022-05-06 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
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2010
- 2010-05-13 CN CN201010178354A patent/CN101825579A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588809A (en) * | 2015-12-15 | 2016-05-18 | 新疆科力新技术发展股份有限公司 | Method for measuring concentration of polyacrylamide in oil field polymer-flooding produced liquid |
| CN107941985A (en) * | 2018-01-12 | 2018-04-20 | 中国海洋石油集团有限公司 | A kind of partially hydrolyzed polyacrylamide (PHPA) suitable for offshore oilfield is birdsed of the same feather flock together the detection method of compound concentration |
| CN108548891A (en) * | 2018-03-13 | 2018-09-18 | 大丰跃龙化学有限公司 | A kind of analysis method detecting polyhexamethylene list guanidine using mixed indicator |
| CN112986052A (en) * | 2019-12-13 | 2021-06-18 | 中国石油天然气股份有限公司 | Method for testing concentration of polyacrylamide and application thereof |
| CN111272612A (en) * | 2020-03-03 | 2020-06-12 | 西南石油大学 | Primary screening method of demulsifier |
| CN111272612B (en) * | 2020-03-03 | 2022-01-28 | 西南石油大学 | Primary screening method of demulsifier |
| CN111595963A (en) * | 2020-04-30 | 2020-08-28 | 中国石油天然气股份有限公司 | Method for measuring hydrolysis degree of partially hydrolyzed polyacrylamide in oil-gas field chemical flooding output fluid |
| CN114441661A (en) * | 2020-11-03 | 2022-05-06 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
| CN114441661B (en) * | 2020-11-03 | 2023-09-12 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
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Open date: 20100908 |