CN106290213A - The detection method of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield - Google Patents
The detection method of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield Download PDFInfo
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- CN106290213A CN106290213A CN201610719299.5A CN201610719299A CN106290213A CN 106290213 A CN106290213 A CN 106290213A CN 201610719299 A CN201610719299 A CN 201610719299A CN 106290213 A CN106290213 A CN 106290213A
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 229920000642 polymer Polymers 0.000 title claims abstract description 65
- 239000007788 liquid Substances 0.000 title claims abstract description 35
- 238000001514 detection method Methods 0.000 title claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 146
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 73
- 238000012360 testing method Methods 0.000 claims abstract description 58
- 238000001471 micro-filtration Methods 0.000 claims abstract description 30
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 12
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 11
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 7
- -1 polypropylene Polymers 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical class ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims 1
- 239000004743 Polypropylene Substances 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- 238000005070 sampling Methods 0.000 abstract description 3
- 238000011835 investigation Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 6
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- OKIIEJOIXGHUKX-UHFFFAOYSA-L Cadmium iodide Inorganic materials [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000011435 rock Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 229940075417 cadmium iodide Drugs 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000014654 dry sauces/powder mixes Nutrition 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229950000845 politef Drugs 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical group O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 description 1
- IZMLBXISTOJVDE-UHFFFAOYSA-M sodium;iodide;hydrate Chemical compound O.[Na+].[I-] IZMLBXISTOJVDE-UHFFFAOYSA-M 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Abstract
The invention discloses the detection method of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield.Including: (1) carries out classification microfiltration pretreatment to sample point sample each in Produced Liquid handling process, obtains the pretreated testing sample of classification microfiltration；(2) the above-mentioned pretreated testing sample of classification microfiltration is carried out total values of nitrogen might (TN), ammonia nitrogen value (NH the most respectively4N), nitrite values of nitrogen might (NO2N), nitrate values of nitrogen might (NO3N) mensuration, uses formula (1) to calculate the apparent polymer values of nitrogen might (PN of testing sample1)；(3) use formula (2) to calculate the actual polymer values of nitrogen might (PN) of testing sample, obtain the actual polymer values of nitrogen might (PN) of testing sample；(4) according to PN C standard curve, the concentration of polymer is determined.The detection method of polymer concentration in the Produced Liquid handling process that the present invention provides, test result is accurate and data reappearance good, while reducing time and Financial cost, the light portable of equipment, demand offshore platform field investigation and sampling can be met, chemically examining on the spot.
Description
Technical field
The invention belongs to quantitative analysis field, be specifically related in a kind of Produced Liquid handling process being suitable to offshore oilfield polymerization
The detection method of substrate concentration.
Background technology
In Produced Liquid handling process, polymer concentration detection is one of marine important job task noting poly-oil field, for referring to
Lead Produced Liquid and process the tracking of each technique unit treatment effect, optimization of process schemes adjustment and treatment agent research and development screening and effect
Fruit is evaluated has important function, is important basic data and theory analysis foundation, and being that impact is poly-drives field test and industrialization
One of key factor of successful implementation.
At present, the used method of offshore oilfield is CdI_2-starch method, bromine water used and glacial acetic acid, tool severe corrosive and
, all there is harm to the healthy of testing staff and environment and pollute in volatility.In order to reduce medicament hazardness, generally require
The main equipments such as fume hood, offshore platform does not the most possess experiment condition.Therefore, " platform sampling-ship fortune can only be used at present
Defeated-land chemical examination " test pattern, there is Financial cost high (relating to logistics transportation and personnel's charge and discharge operations) and poor in timeliness
The problem of (the detection cycle was up to 20～40 days).The particularity of offshore platform, it is desirable to polymer concentration in Produced Liquid handling process
Detection method answers accurate quick, equipment needed thereby volume little, lightweight, can directly carry or be placed on platform, with satisfied scene
Sampling, the demand chemically examined on the spot.
The polymer output concentration that the author's early-stage Study is set up " determines nitrogen " or " micro-filtration membrane-the determine nitrogen " rapid assay methods (phase
Periodical paper oilfield chemistry, 2016,33 (1): 176-180, patent 201410775942.7 and 201410776568.2) method has
Strong, the cost reduction portable, ageing of effect, instrument, is applied to injection end and extraction well head polymer Concentration Testing, presents good
Effect of field application.But when the method is applied to polymer concentration detection in Produced Liquid handling process, find that detection is accurately
Property and precision reduce problem.Analyze its reason, may have a following two aspect: sample composition in (1) Produced Liquid handling process
More complicated, remove containing impurity such as microorganism, oils, solid suspensions, may be possibly together with all kinds of chemical treatment medicaments and medicament
The interfering materials such as the floc sedimentation produced when playing a role.(2) liquid source is more complicated and changeable, and the liquid of Produced Liquid handling process comes
Source is the mixing liquid of each extraction well head substantially, affects testing result, in turn results in polymer concentration detection data distortion.
Therefore, polymer in the Produced Liquid handling process being suitable to offshore oilfield of a kind of quick high accuracy and precision is set up
Concentration detection method is the most necessary.
Summary of the invention
Present invention seek to address that existing detection method operation complexity, poor in timeliness, reagent toxic and volatile, error relatively greatly,
The problems such as data reappearance difference, it is provided that the detection side of polymer concentration in a kind of Produced Liquid handling process being suitable to offshore oilfield
Method.
The detection method of polymer concentration in the Produced Liquid handling process being suitable to offshore oilfield provided by the present invention, including
Following step:
(1) sample point sample each in Produced Liquid handling process is carried out classification microfiltration pretreatment, obtain classification microfiltration and locate in advance
Testing sample after reason；
(2) the above-mentioned pretreated testing sample of classification microfiltration is carried out total values of nitrogen might (TN), ammonia nitrogen value (NH the most respectively4-
N), nitrite values of nitrogen might (NO2-N), nitrate values of nitrogen might (NO3-N) mensuration, use following formula (1) calculate testing sample apparent
Polymer values of nitrogen might (PN1):
PN1=TN-(NH4-N)-(NO2-N)-(NO3-N) formula (1)；
(3) using following formula (2) to calculate the actual polymer values of nitrogen might (PN) of testing sample, the reality obtaining testing sample is gathered
Compound values of nitrogen might (PN):
PN=PN1-PN0Formula (2)；
In formula (2), PNoRepresent background values of nitrogen might；
(4) according to PN-C standard curve, the concentration of polymer in described testing sample is determined.
In said method step (1), the concrete operations of described classification microfiltration are: to sample point each in Produced Liquid handling process
Sample carries out repeatedly microfiltration pretreatment, with by the solid suspension in each sample point production fluid, oils, antibacterial, all kinds of floc sedimentations etc.
Impurity retains completely, and polymer all passes through with water, it is to avoid measure time error interference.
Described microfiltration specifically can be carried out twice, and wherein microfiltration can be selected for the microfiltration that range of aperture size is 2-5 μm for the first time
Film, microfiltration can be selected for the micro-filtration membrane that aperture size is 0.2-1 μm for the second time.
Described micro-filtrate membrane filtration, specifically can plug micro-filtration membrane needle-based filter by drawing described production fluid with syringe
Device, manual injection device realizes filtering, and the diameter of described filter can be 20～50mm；The material of described micro-filtration membrane be polyether sulfone,
Any one in acetate fiber, polyacrylonitrile, politef, Kynoar and nylon.
In said method step (2), described total values of nitrogen might (TN), ammonia nitrogen value (NH4-N), nitrite values of nitrogen might (NO2-N), nitre
Hydrochlorate values of nitrogen might (NO3-N) all use UV-VIS spectrophotometry to be measured.
In said method step (3), described background values of nitrogen might PNoDetermined by following method:
Collect all treatment agents in Produced Liquid flow process, use on-the-spot injection allocation water, prepare according to platform field injection allocation concentration
Solution, uses method described in step (2) to detect total values of nitrogen might (TN ') of prepared solution, ammonia nitrogen value (NH the most respectively4-
N '), nitrite values of nitrogen might (NO2-N '), nitrate values of nitrogen might (NO3-N '), use following formula (3) to calculate background values of nitrogen might PN0；
PN0=TN'-(NH4-N')-(NO2-N')-(NO3-N') formula (3)
Wherein, described treatment agent includes water cleaning agent, flocculant, defoamer, corrosion inhibiter, preservative, demulsifier, antibacterial
And other chemical agents.
In said method step (4), described PN-C standard curve is set up by the method comprised the steps:
A () uses on-the-spot injection allocation water, prepare at least 5 variable concentrations (CKnown) Polymer Standards aqueous solution；
B () uses method described in step (2) to detect the Polymer Standards water of above-mentioned at least 5 variable concentrations the most respectively
Total values of nitrogen might of solution (TN "), ammonia nitrogen value (NH4-N "), nitrite values of nitrogen might (NO2-N "), nitrate values of nitrogen might (NO3-N "), use
Following formula (4) calculates polymer values of nitrogen might PN "
PN "=TN "-(NH4-N")-(NO2-N")-(NO3-N ") formula (4)
C () is with the polymer concentration C of the Polymer Standards aqueous solution of above-mentioned at least 5 variable concentrationsKnownFor abscissa, with
Polymer values of nitrogen might PN of the Polymer Standards aqueous solution of above-mentioned at least 5 variable concentrations " it is vertical coordinate, draw PN-C standard bent
Line, and simulate linear equation；
In step (a), described polymer is partially hydrolyzed polyacrylamide (PHPA)；
The molecular weight of described partially hydrolyzed polyacrylamide (PHPA) is 800～28,000,000, concretely 17,000,000；Degree of hydrolysis is
10%～50%, concretely 37%.
The concentration of described Polymer Standards aqueous solution is 0～500mg/L, concretely 0,20,40,60,80,100,120,
140、160、180、200、220、240、260、280、300mg/L。
Described Polymer Standards aqueous solution can be obtained by polymer mother liquor dilution；Described polymer mother liquor is by Polymer Standards
Product obtain through standing overnight after mixing with Oil Field injection allocation water, specifically can be by being existed by Polymer Standards product (polymer dry powder)
Joining agitated in on-the-spot injection allocation water obtaining at a temperature of Oil Field injection allocation, described mixing speed can be 300～500rpm；
The concentration of described polymer mother liquor can be 5000～10000mg/L, concretely 5000mg/L.
In step (c), described linear equation concretely PN=C/7.84.
In above-mentioned detection method, if the concentration of polymer is more than 500mg/L in described testing sample, can be certain by dilution
Multiple, by concentration regulation to the range of linearity, specifically can dilute 2～10 times.
Design portable test device (schematic diagram is as shown in Figure 1) based on said method, mainly include portable spectrophotometric
Meter, heating digestion device, micro-filtration membrane syringe filter, total nitrogen test kit, nitrate nitrogen test kit, nitrite nitrogen test agent
8 parts such as box, ammonia nitrogen test kit, quantitative liquid shifter, equipment volume is little (is about 100cm, width about 50cm, high about
40cm), lightweight (nearly weighing 5kg), portability to offshore platform uses.
The detection method of polymer concentration in Produced Liquid handling process provided by the present invention, takes into full account and eliminates each
Item interference factor, test result is accurate and data reappearance good.
The technology of the present invention is simple to operate, and equipment is the most portable, the need can meet offshore platform field investigation and sampling, chemically examining on the spot
Ask, meanwhile significantly reduce the time cost that polymer concentration is evaluated, offshore oilfield traditional starch-cadmium iodide method detection cycle
20-40 days/batches, and ＜ of the present invention 0.5 day/crowd, time shortening 400-800 times, be significantly reduced Financial cost simultaneously, compared
4-5 times is declined compared with traditional starch-cadmium iodide method each sample detection cost.
Accompanying drawing explanation
Fig. 1 be the present invention Produced Liquid handling process in polymer concentration detection equipment schematic diagram, wherein, 1 is portable
Formula spectrophotometer, 2 is heating digestion device, and 3 is micro-filtration membrane syringe filter, and 4 is total nitrogen test kit, and 5 test for nitrate nitrogen
Test kit, 6 is nitrite nitrogen test kit, and 7 is ammonia nitrogen test kit, and 8 is quantitative liquid shifter.
Detailed description of the invention
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental technique used in following embodiment if no special instructions, is conventional method；Institute in following embodiment
Reagent, material etc., if no special instructions, the most commercially obtain.
In following embodiment, the mensuration of total values of nitrogen might completes based on total nitrogen test kit, and test kit includes special colorimetric
Pipe and tri-kinds of reagent of TN-1, TN-2, TN-3.Being 5ml deionized water in special color comparison tube, TN-1, TN-2, TN-3 reagent is respectively
Potassium peroxydisulfate powder, sodium hydroxide solution (0.5g/L) and hydrochloric acid solution (0.2g/L).During test, first by portable light splitting light
Degree meter is adjusted to total nitrogen test mode, blank compared with zero after standby.Then, toward empty test tube is sequentially added into 1.0ml sample,
9ml water, 0.5gTN-1 reagent, after mix homogeneously, add 1mlTN-2 reagent, screw cap, clear up in digestion device, temperature
120 DEG C, 60 minutes time, after having cleared up, empty test tube is taken out, draws wherein 1.0ml sample, join special color comparison tube
In, it is subsequently adding 1.0ml TN-3 reagent, screws cap, rock mixing, after reacting 10 minutes, special color comparison tube is inserted into just
Take in formula spectrophotometer, read total nitrogen numerical value；
The mensuration of ammonia nitrogen value completes based on ammonia nitrogen test kit, and test kit includes special color comparison tube, NH4-N-1 tries
Agent, equipped with the nessler reagent (mercuric iodixde-potassium iodide-sodium hydroxide solution) of 5.0ml, NH in special color comparison tube4-N-1 reagent is
Sodium potassium tartrate tetrahydrate pressed powder.During test, first portable spectrophotometer is adjusted to ammonia nitrogen test mode, blank complete compared with zero
Finish rear standby.In special color comparison tube, drip 0.5ml sample mix homogeneously, add the NH of 0.5g4-N-1 reagent, rock so that
Solid matter dissolves, and after reacting 15 minutes, inserts spectrophotometer, reads ammonia nitrogen value；
Nitrite values of nitrogen might (NO2-N) mensuration complete based on nitrite nitrogen test kit, test kit includes specially
With color comparison tube and NO2-N-1 reagent, solid equipped with P-aminobenzene-sulfonamide, hydrochloric acid N-(1-naphthalene)-ethylenediamine etc. in special color comparison tube
Body powder, NO2-N-1 reagent is hydrochloric acid solution.During test, first portable spectrophotometer is adjusted to nitrite nitrogen and surveys
Examination state, blank compared with zero after standby.In special color comparison tube, drip 5ml sample, add 1 NO2-N-1 reagent, firmly shakes
Moving makes solid matter dissolve, and after reacting 10 minutes, inserts spectrophotometer, reads nitrite nitrogen；
Nitrate values of nitrogen might (NO3-N) mensuration complete based on nitrate nitrogen test kit, test kit includes special ratio
Colour tube and NO3-N-1 reagent, equipped with disulfonic acid phenol reagent, NO in special color comparison tube3-N-1 reagent is sodium carbonate liquor.During test,
First portable spectrophotometer is adjusted to nitrate nitrogen test mode, blank compared with zero after standby.Toward special color comparison tube
Middle addition 0.5g NO3-N-1 reagent, rocks, and adds 2.0ml water sample immediately, screws pipe cap mixing, firmly rocks, react 30 points
Zhong Hou, inserts spectrophotometer, reads nitrate nitrogen.
Polymer concentration detection in embodiment, Bohai Sea A oil field mining liquid handling process
(1) standard curve is set up:
50 DEG C, under the conditions of 400rpm by scene partially hydrolyzed polyacrylamide (PHPA) (degree of hydrolysis be molecular weight be 12,000,000, water
Solution degree 37%) dry powder mixes with on-the-spot injection allocation water, stands overnight, obtain 5000mg/L mother solution after being completely dissolved.Mother solution is on-the-spot
Injection allocation water be diluted to concentration be respectively 0,20,40,60,80,100,120,140,160,180,200,220,240,260,280,
The polyacrylamide standard aqueous solution of 300mg/L.UV-VIS spectrophotometry is used to detect total values of nitrogen might of water sample the most respectively
TN, ammonia nitrogen value Na, nitrite nitrogen Nb, nitrate nitrogen Nc, calculate polymer nitrogen PN value.It is horizontal seat with polymer concentration C (mg/L)
Mark, with polymer values of nitrogen might PN (mg/L) as vertical coordinate, draws PN-C standard curve, and to simulate linear equation is PN=C/
7.84。
(2) background values of nitrogen might PNoDetermine
Collect all treatment agents in Produced Liquid flow process (include water cleaning agent, flocculant, defoamer, corrosion inhibiter, preservative,
Demulsifier, antibacterial etc.), use on-the-spot injection allocation water, use UV-VIS spectrophotometry to detect the total nitrogen of water sample the most respectively
Value (TN '), ammonia nitrogen value (NH4-N '), nitrite values of nitrogen might (NO2-N '), nitrate values of nitrogen might (NO3-N '), calculate background nitrogen
Value PNo, result is as shown in table 1.Table 1 is the corresponding table of the background values of nitrogen might that treatment agent used causes with it in Produced Liquid flow process.
The corresponding table of the background values of nitrogen might that treatment agent used causes with it in table 1 Produced Liquid flow process
As shown in Table 1, total background values of nitrogen might PNoValue is 0.154mg/L.
(3) polymer concentration detection in Produced Liquid handling process
First sample point sample each in Produced Liquid handling process carries out classification microfiltration pretreatment, and (it is micro-that twice microfiltration processes
Filter sizes is respectively 2 μm and 0.45 μm).Then UV-VIS spectrophotometry is used to detect total values of nitrogen might of water sample the most respectively
(TN), ammonia nitrogen value (NH4-N), nitrite values of nitrogen might (NO2-N), nitrate values of nitrogen might (NO3-N), use formula (1) to calculate testing sample
Apparent polymer values of nitrogen might (PN1), use formula (2) to calculate the actual polymer values of nitrogen might (PN) of testing sample.Obtain testing sample
Actual polymer values of nitrogen might (PN) after, obtain the concentration of described polymer in described testing sample according to PN-C linear equation,
Test result is as shown in the table.Use the detection of starch cadmium iodide method simultaneously, compare the accuracy of data.Table 2 is for using this
The polymer concentration value that bright method and CdI_2-starch method measure.
Table 2 uses the polymer concentration value that the inventive method and CdI_2-starch method measure
As shown in Table 2, data result and CdI_2-starch method measure polymer concentration value in the range of error allows,
Maintaining preferable concordance, method is accurately and reliably.
Claims (7)
1. be suitable to a detection method for polymer concentration in the Produced Liquid handling process of offshore oilfield, comprise the steps:
(1) sample point sample each in Produced Liquid handling process is carried out classification microfiltration pretreatment, after obtaining classification microfiltration pretreatment
Testing sample；
(2) the above-mentioned pretreated testing sample of classification microfiltration is carried out total values of nitrogen might (TN), ammonia nitrogen value (NH the most respectively4-N), sub-
Nitrate values of nitrogen might (NO2-N), nitrate values of nitrogen might (NO3-N) mensuration, use following formula (1) calculate testing sample apparent polymerization
Thing values of nitrogen might (PN1):
PN1=TN-(NH4-N)-(NO2-N)-(NO3-N) formula (1)；
(3) use following formula (2) to calculate the actual polymer values of nitrogen might (PN) of testing sample, obtain the actual polymer of testing sample
Values of nitrogen might (PN):
PN=PN1-PN0Formula (2)；
In formula (2), PNoRepresent background values of nitrogen might；
(4) according to PN-C standard curve, the concentration of polymer in described testing sample is determined.
Method the most according to claim 1, it is characterised in that: in step (1), the operation of described classification microfiltration is: to adopting
Go out each sample point sample in liquid handling process and carry out repeatedly microfiltration pretreatment；
Described microfiltration is carried out twice, the micro-filtration membrane that wherein microfiltration selects range of aperture size to be 2-5 μm for the first time, microfiltration for the second time
Select the micro-filtration membrane of aperture a size of 0.2-1 μm.
Method the most according to claim 1 and 2, it is characterised in that: in step (2), described total values of nitrogen might (TN), ammonia nitrogen value
(NH4-N), nitrite values of nitrogen might (NO2-N), nitrate values of nitrogen might (NO3-N) all use UV-VIS spectrophotometry to be measured.
4. according to the method according to any one of claim 1-3, it is characterised in that: in step (3), described background values of nitrogen might PNoLogical
Cross following method to determine:
Collect all treatment agents in Produced Liquid flow process, use on-the-spot injection allocation water, prepare solution according to platform field injection allocation concentration,
Use method described in step (2) to detect total values of nitrogen might TN of prepared solution the most respectively ', ammonia nitrogen value NH4-N ', nitrous acid
Salt values of nitrogen might NO2-N ', nitrate values of nitrogen might NO3-N ', uses following formula (3) to calculate background values of nitrogen might PN0；
PN0=TN'-(NH4-N')-(NO2-N')-(NO3-N') formula (3).
5. according to the method according to any one of claim 1-4, it is characterised in that: in step (4), described PN-C standard curve
Set up by the method comprised the steps:
A () uses on-the-spot injection allocation water, prepare at least 5 variable concentrations CKnownPolymer Standards aqueous solution；
B () uses method described in step (2) in claim 1 to detect the polymerization of above-mentioned at least 5 variable concentrations the most respectively
Total values of nitrogen might TN of thing standard aqueous solution ", ammonia nitrogen value NH4-N ", nitrite values of nitrogen might NO2-N ", nitrate values of nitrogen might NO3-N ", use
Following formula (4) calculates polymer values of nitrogen might PN ":
PN "=TN "-(NH4-N")-(NO2-N")-(NO3-N ") formula (4)
C () is with the polymer concentration C of the Polymer Standards aqueous solution of above-mentioned at least 5 variable concentrationsKnownFor abscissa, with above-mentioned
Polymer values of nitrogen might PN of the Polymer Standards aqueous solution of at least 5 variable concentrations " it is vertical coordinate, draw PN-C standard curve, and
Simulate linear equation.
Method the most according to claim 5, it is characterised in that: in step (a), described polymer is partial hydrolysis polypropylene
Amide；
The molecular weight of described partially hydrolyzed polyacrylamide (PHPA) is 800～28,000,000；Degree of hydrolysis is 10%～50%；
The concentration of described Polymer Standards aqueous solution is 0～500mg/L.
7. according to the method according to any one of claim 1-6, it is characterised in that: in described method, if described testing sample
The concentration of middle polymer is more than 500mg/L, and by dilution certain multiple by concentration regulation to the range of linearity, extension rate is 2
～10 times.
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| CN112304827A (en) * | 2020-04-07 | 2021-02-02 | 中国石油天然气股份有限公司 | Method and device for obtaining content of polymer microspheres in oil field output liquid |
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| 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 |
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| CN112304827B (en) * | 2020-04-07 | 2024-02-02 | 中国石油天然气股份有限公司 | Method and device for obtaining content of polymer microspheres in oil field produced liquid |
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