CN108693073A - A kind of residual oil salt content assay method - Google Patents
A kind of residual oil salt content assay method Download PDFInfo
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- CN108693073A CN108693073A CN201810804930.0A CN201810804930A CN108693073A CN 108693073 A CN108693073 A CN 108693073A CN 201810804930 A CN201810804930 A CN 201810804930A CN 108693073 A CN108693073 A CN 108693073A
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- 150000003839 salts Chemical class 0.000 title claims abstract description 324
- 238000003556 assay Methods 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 318
- 238000010790 dilution Methods 0.000 claims abstract description 101
- 239000012895 dilution Substances 0.000 claims abstract description 101
- 239000004148 curcumin Substances 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005553 drilling Methods 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 70
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 48
- 235000019441 ethanol Nutrition 0.000 claims description 47
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 46
- 238000001914 filtration Methods 0.000 claims description 39
- 238000002347 injection Methods 0.000 claims description 39
- 239000007924 injection Substances 0.000 claims description 39
- 239000012153 distilled water Substances 0.000 claims description 38
- 239000012530 fluid Substances 0.000 claims description 38
- 238000005259 measurement Methods 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 35
- 238000001514 detection method Methods 0.000 claims description 29
- 239000000284 extract Substances 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- 235000015927 pasta Nutrition 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 26
- 238000000861 blow drying Methods 0.000 claims description 26
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 24
- 238000012360 testing method Methods 0.000 claims description 24
- 230000010076 replication Effects 0.000 claims description 23
- 238000005119 centrifugation Methods 0.000 claims description 16
- 239000003792 electrolyte Substances 0.000 claims description 15
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000007865 diluting Methods 0.000 claims description 13
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 12
- 230000005499 meniscus Effects 0.000 claims description 12
- 238000004062 sedimentation Methods 0.000 claims description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 12
- 235000011152 sodium sulphate Nutrition 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 11
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 11
- 230000005611 electricity Effects 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 238000007792 addition Methods 0.000 claims description 7
- 239000002893 slag Substances 0.000 claims description 4
- 241000370738 Chlorion Species 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 239000013589 supplement Substances 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- 238000004140 cleaning Methods 0.000 claims 1
- 239000006210 lotion Substances 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004939 coking Methods 0.000 abstract description 2
- 230000001934 delay Effects 0.000 abstract description 2
- 230000003111 delayed effect Effects 0.000 abstract description 2
- 238000005868 electrolysis reaction Methods 0.000 description 15
- 238000004448 titration Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000004519 grease Substances 0.000 description 11
- 238000010998 test method Methods 0.000 description 11
- 239000011259 mixed solution Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000003869 coulometry Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- 241000208195 Buxaceae Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- QSDSNNSKORVORL-UHFFFAOYSA-N acetic acid;silver Chemical compound [Ag].CC(O)=O QSDSNNSKORVORL-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Process provides a kind of residual oil salt content assay method, technical solution is to include the following steps:It will be stirred evenly after residual oil heating and melting to be measured, measure the numerical value E1 of its 100 DEG C of Engler viscosity, when being spent more than 10 conditions such as E1, addition white oil is needed to be diluted, it is uniformly mixed, by E100 DEG C of Engler viscosity control between 2-10 condition degree, with salt content in residual oil after alcohol-water mixture extracting dilution, with salt content in small-hole drilling or Potentiometric Determination residual oil, the white oil, which uses, is free of inorganic salts white oil.Advantageous effect is:The invention enables using and detecting, residual oil more science is accurate, effective raising can be obtained in control of product quality level, to the stable operation of delayed coking unit, delays equipment corrosion rate, extends device and pipeline service life, improve product quality and have vital effect.
Description
Technical field
The present invention relates to a kind of residual oil detection method, more particularly to a kind of residual oil salt content assay method.
Background technology
Currently, China does not measure the national standard and petrochemical industry standard of residual oil salt content, since residual oil viscosity is excessive, salt
Content can not be measured directly.It is consulted by pertinent literature and experiment is groped, the detection method of residual oil salt content mainly has following two
Kind mode:Coulometry and the direct combustion method of coulomb;1)Coulometry
Sample heats in the presence of a polar solvent, extracts salt wherein included with water, is extracted in right amount with syringe after centrifugation
Extract injects in the acetic acid electrolyte containing a certain amount of silver ion, and the chlorion in sample reacts with silver ion, reacts
The silver ion of consumption is given birth to by generation electrode electricity and is supplemented, and by measuring the electricity of the raw silver ion consumption of electricity, is according to Faraday's law
Sample salt content can be acquired, but residual oil viscosity is excessive, salt wherein included can not be extracted with water, the method can not measure its salt and contain
Amount.
2)The direct combustion method of coulomb:Directly reactant is injected in cracking tube with solid sampler, burns, fires at high temperature
It burns product and passes through N2And O2Mixed gas bring into titration cell, measure the content of total chlorine, but content of organic chloride can not be measured, institute
Its salt content can not be measured in this approach.
Invention content
The purpose of the present invention provides a kind of residual oil salt content measurement side aiming at drawbacks described above of the existing technology
Method, by the way that residual oil to be measured to be diluted with white oil, and by E100(100 DEG C of Engler viscosity)It controls between 2-10 condition degree,
It may make with salt content in small-hole drilling or Potentiometric Determination residual oil with salt content in residual oil after alcohol-water mixture extracting dilution
It is accurate to use and detect residual oil more science, delays equipment corrosion rate, extend device and pipeline service life.
A kind of residual oil salt content assay method that the present invention mentions, includes the following steps:After residual oil heating and melting to be measured
It stirs evenly, measures the numerical value E1 of its 100 DEG C of Engler viscosity, when being spent more than 10 conditions such as E1, addition white oil is needed to be diluted,
It is uniformly mixed, by E100 DEG C of Engler viscosity control between 2-10 condition degree, with salt in residual oil after alcohol-water mixture extracting dilution
Content, with salt content in small-hole drilling or Potentiometric Determination residual oil,
The white oil, which uses, is free of inorganic salts white oil.
Preferably, a kind of residual oil salt content assay method that the present invention mentions, carries out as follows:
A, the measurement of residual oil Engler viscosity to be measured;B, after dilution the salt content of residual oil measurement;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
The quality of the white oil without inorganic salts, g is added in m2---.
Wherein, the measurement of a residual oil Engler viscosity to be measured includes the following steps:
A1, residual oil to be measured is heated to 100-110 DEG C, and stirred evenly;
A2, instrument heating is opened, opening blender first will be wooden when instrument outer container fluid temperature reaches 99.8-100.2 DEG C
Plug tightly clogs the tap hole of viscosimeter, then will be previously heated in the residual oil injection inner pressurd vessel of a little higher than set point of temperature, note
The tip of the necessary a little higher than spike of pasta entered;When thermometer in sample reaches set point of temperature just, then 5min is kept, it is just fast
Speed lifts stopper, while starting stopwatch, when the sample in receiving flask is right up to the graticule of 200mL, reads the outflow of sample
Time T1;
A3 while the water number for measuring Engler viscometer are that distilled water flows out the time needed for 200mL at 20 DEG C from viscosimeter
T2;
A4, residual oil Engler viscosity are calculated as follows:E100=T1/T2
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s.
B, the measurement of the salt content of residual oil, includes the following steps after dilution:
B1, the numerical value E1 for measuring 100 DEG C of Engler viscosity of residual oil to be measured, when spending more than 10 conditions such as E1, need to take residual oil to be measured
100-120g is added the white oil without inorganic salts and is diluted, and is uniformly mixed, by 100 DEG C of Engler viscosity controls in 2-10 condition degree
Between, and the quality m1 of residual oil and addition are free of the quality m2 of the white oil of inorganic salts when accurate recording dilution;
B2, the residual oil after dilution is heated to 50--70 DEG C, then stirs evenly sample, and quickly take 0.8-1.2g oil samples in
In centrifuge tube, 1.5ml dimethylbenzene, 2.0ml alcohol-aqueous solution is added;
B3, centrifuge tube is put into 70~80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheated
1 minute, then shaken 1 minute with flash mixer, it is then placed in centrifuge, 1~2 is centrifuged under 2000~3000rpm rotating speeds
Minute, it is apparent two-phase to make water-oil separating;
B4, Microcoulomb instrument is opened, after connecting electrolytic cell, mixes up bias, after baseline is steady plus salt standard specimen measures average transformation
Rate is advisable between 75%-100%;
B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then air is injected 1~2 time with a 0.25ml syringe,
The oil discharge that will enter in syringe needle, then extracts a small amount of extracting solution, micro syringe and syringe needle 2~3 times is rinsed, then with micro
0.2ml samples are added to electrolytic cell in syringe, are repeated three times, and measure the salt content X1 that is averaged in residual oil after diluting;
B6 and then selection and standard specimen similar in sample to be tested, a concentration of X2 carry out reactionary slogan, anti-communist poster, measure the salt content X3 of standard specimen;
B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content X0 in blank;
The salt content of residual oil is calculated as follows after b8, dilution:A salt=((X1-X0)*X2)/X3
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L.
Before measuring viscosity every time, the inner pressurd vessel and its effuser of viscosimeter are carefully washed with the clean solvent oil of filtration, so
Use air blow drying, the inaccurate wiping of inner pressurd vessel that the filter paper with edge of having one's hair trimmed only is allowed to suck remaining drop afterwards.
Preferably, when salt content measures in the residual oil excessively high to sulfide content, 1 drop 30%H is added2O2, to eliminate interference,
If 30% H is added2O2, take 2ml water samples in centrifuge tube in b3 steps, heated in 70 DEG C of water-baths 1 minute, 1 drop is then added
30% H2O2, wait for that water sample is cooled to room temperature after being vigorously mixed and analyzed.
Preferably, when salt content measures, by treated, sample injects in the acetic acid electrolyte containing silver ion, sample
In chlorion i.e. react with silver ion:Cl-+Ag+→ AgCl↓
The silver ion for reacting consumption gives birth to supplement by generation electrode electricity, by measuring the electricity of the raw silver ion consumption of electricity, according to farad
Law can acquire salt content.
Salt content detection limit of the present invention:2.0mg/L-10000mg/L higher than being detected after can the diluting sample of the upper limit.
The beneficial effects of the invention are as follows:It is accurate that the present invention uses and detect residual oil more science, has delayed the corrosion of equipment
Speed extends device and pipeline service life, by the way that residual oil to be measured to be diluted with white oil, and by E100(100 DEG C of engler
Viscosity)Control is between 2-10 condition degree, salt content in residual oil after being diluted with alcohol-water mixture extracting, with small-hole drilling or current potential
Method measures salt content in residual oil;The invention enables using and detecting residual oil quality control level effective raising can be obtained, to prolonging
The stable operation of slow coking plant, raising product quality have vital effect, have filled up national nothing and have accurately measured residual oil
The blank of salt content.
Description of the drawings
Attached drawing 1 is the structural schematic diagram of the electrolytic cell of the present invention;
Attached drawing 2 is the structural schematic diagram of the Engler viscosity analyzer of the present invention;
In upper figure:Electrolytic anode 1, reference electrode 3, measuring electrode 4, reference chamber 5, the first amberplex 6, stirs electrolysis cathode 2
Mix son 7, anode chamber 8, the second amberplex 9, cathode chamber 10;
Stopper jack a1, stopper a2, blender a3, receiving flask a4, horizontal adjustment screw a5, tap hole a6, spike a7, spheric
Bottom a8, metal tripod a9, inner pressurd vessel a10, thermowell a11, outer container a12.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 105 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 4946s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=4946s/51s=96.98;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)96.98 condition degree of numerical value, because E100 be more than 10 condition degree, take
White oil is added in residual oil 100g to be measured(Without inorganic salts)66.7g is diluted, and 30min is stirred using explosion-proof blender, by above-mentioned
A2 steps are tested, and the residual oil E100 after dilution is measured(100 DEG C of Engler viscosity)For 6.16 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 0.82g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;
B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from left to right successively
Reference electrode 3, measuring electrode 4, electrolytic anode 1, electrolysis cathode 2 are connected on the binding post of titration cell, 7 turns of stirrer is adjusted
It is dynamic steady, and pay attention to being protected from light, with reference to attached drawing 1, after connecting electrolytic cell, bias is mixed up, salt content standard specimen is added after baseline is steady
It is 87.5% to measure average conversion;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml
Emitter injects air 2 times, and the oil entered in syringe needle is discharged, a small amount of extracting solution is then extracted, rinses micro syringe and syringe needle 3
It is secondary, it then uses micro syringe that 0.2ml samples are added to electrolytic cell, is repeated three times, measure after dilution average salt in residual oil
Content 4.328mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, standard specimen is measured
Salt content 5.03mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;It is b8, dilute
The salt content for releasing rear residual oil is calculated as follows:A salt=((X1-X0)*X2)/X3=4.302mg/L
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=7.171mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
With reference to attached drawing 1, the electrolytic cell that the present invention mentions(Also referred to as titration cell), including one reference electrode pair of instruction and electrolysis sun
One cathode electrode pair of pole.Wherein, one reference electrode of instruction is to the variation for measuring concentration of silver ions, including reference electrode 3, survey
Measure electrode 4, reference chamber 5, the first amberplex 6;One cathode electrode of electrolytic anode is to for keeping silver constant in electrolyte
Ion concentration, including electrolytic anode 1, electrolysis cathode 2, the second amberplex 9, cathode chamber 10;Wherein measuring electrode 4 is silver-colored electricity
Pole, reference electrode 3 are a silver-colored acetic acid silver electrodes;Electrolytic anode 1 is silver electrode, and electrolysis the moon 2 is platinum electrode.
With reference to attached drawing 2, Engler viscosity analyzer of the invention includes the inner pressurd vessel a10 for filling sample, and it is effective to block outflow
Stopper a2, metal tripod a9, the inner pressurd vessel a10 for containing sample are installed in the outer container a12 for being used as water-bath or oil bath, the two
Container is all manufactured with brass, and the bottom of inner pressurd vessel is spherical bottom a8, and inner surface will pass through polishing and gold-plated.Inner pressurd vessel is equipped with Huang
Hollow convex lid made of copper is covered with stopper jack a1 and thermowell a11, is used for being inserted into stopper and thermometer;
Stopper is the tap hole a6 for blocking instrument.
In inner pressurd vessel, with equidistant, installation is made there are three spike a7 at a right angle is bent up on wall from bottom
The indicator of fuel head and instrument level in order to control.Blender a3 and thermometer are equipped in outer container, this thermometer utilizes
Clip in outer container wall is fixed on three steady arms and effuser in outer container to fix interior objective device.Effuser will utilize
A2 stoppers by covering centre bore block up.This stopper is made of hardwood (boxwood and other), for placing instrument
Metal tripod a9 is made of a circle and the long foot of item, wherein there is two feet that horizontal adjustment screw a5, metal is arranged
Receiving flask a4 is installed in tripod a9.
Embodiment 2:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 103 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 7402s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=7402s/51s=145.14;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)145.14 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 105.3g to be measured that white oil is added(Without inorganic salts)70.0g is diluted, and is stirred 30min using explosion-proof blender, is pressed
Above-mentioned a2 steps test, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 7.88 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 0.97g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;
B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from left to right successively
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post, stirrer stability of rotation is adjusted,
And pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, after baseline is steady plus salt content standard specimen measures average conversion and is
80.6%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then air is injected 2 times with a 0.25ml syringe,
The oil discharge that will enter in syringe needle, then extracts a small amount of extracting solution, micro syringe and syringe needle 3 times is rinsed, then with micro note
0.2ml samples are added to electrolytic cell in emitter, are repeated three times, and measure the salt content 1.232mg/L that is averaged in residual oil after diluting;
B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt content 4.96mg/ of standard specimen is measured
L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;
The salt content of residual oil is calculated as follows after b8, dilution:A salt=((X1-X0)*X2)/X3=1.242mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=2.068mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 3:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 105 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 17944s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during the test;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=17944s/51s=351.84;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)351.84 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 110g to be measured that white oil is added(Without inorganic salts)110g is diluted, and 30min is stirred using explosion-proof blender, by above-mentioned
A2 steps are tested, and the residual oil E100 after dilution is measured(100 DEG C of Engler viscosity)For 5.92 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 1.05g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;
B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from left to right successively
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post, stirrer stability of rotation is adjusted,
And pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, after baseline is steady plus salt content standard specimen measures average conversion and is
90.9%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then air is injected 2 times with a 0.25ml syringe,
The oil discharge that will enter in syringe needle, then extracts a small amount of extracting solution, micro syringe and syringe needle 3 times is rinsed, then with micro note
0.2ml samples are added to electrolytic cell in emitter, are repeated three times, and measure the salt content 3.733mg/L that is averaged in residual oil after diluting;
B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt content 5.01mg/ of standard specimen is measured
L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;
The salt content of residual oil is calculated as follows after b8, dilution:A salt=((X1-X0)*X2)/X3=3.726mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=7.452mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 4:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 100 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 7384s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=7384s/51s=144.78;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)144.78 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 101.2g to be measured that white oil is added(Without inorganic salts)67.5g is diluted, and is stirred 30min using explosion-proof blender, is pressed
Above-mentioned a2 steps test, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 7.84 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 1.01g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 79.9%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
8.036mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 5.00mg/L;
B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;
The salt content of residual oil is calculated as follows after b8, dilution:A salt=((X1-X0)*X2)/X3=8.036mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=13.396mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 5:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
The test method carries out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 107 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 14284s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during the test;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=14284s/51s=280.07;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)280.07 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 106.9g to be measured that white oil is added(Without inorganic salts)106.9g is diluted, and is stirred 30min using explosion-proof blender, is pressed
Above-mentioned a2 steps test, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 5.29 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 0.89g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 95.1%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
7.877mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 5.06mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;After b8, dilution
The salt content of residual oil is calculated as follows:A salt=((X1-X0)*X2)/X3=7.784mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=15.568mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 6:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 105 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 13707s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during the test;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=13707s/51s=268.76;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)268.76 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 109g to be measured that white oil is added(Without inorganic salts)109g is diluted, and 30min is stirred using explosion-proof blender, by above-mentioned
A2 steps are tested, and the residual oil E100 after dilution is measured(100 DEG C of Engler viscosity)For 5.18 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 1.10g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 84.1%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
17.099mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 4.95mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;After b8, dilution
The salt content of residual oil is calculated as follows:A salt=((X1-X0)*X2)/X3=17.272mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=34.544mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 7:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 102 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 14974s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during the test;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=14974s/51s=293.61;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)293.61 condition degree of numerical value, because E100 be more than 10 condition degree,
Take residual oil 100.7g to be measured that white oil is added(Without inorganic salts)100.7g is diluted, and is stirred 30min using explosion-proof blender, is pressed
Above-mentioned a2 steps test, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 5.41 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 0.85g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 96.4%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
6.27mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt for measuring standard specimen contains
Measure 5mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;Residual oil after b8, dilution
Salt content be calculated as follows:A salt=((X1-X0)*X2)/X3=6.27mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=12.54mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 8:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 110 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 3773s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=3773s/51s=73.98;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)73.98 condition degree of numerical value, because E100 be more than 10 condition degree, take
White oil is added in residual oil 104.3g to be measured(Without inorganic salts)69.5g is diluted, and 30min is stirred using explosion-proof blender, by upper
It states a2 steps to be tested, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 5.22 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 1.10g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 81.3%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
4.235mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 5.02mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;After b8, dilution
The salt content of residual oil is calculated as follows:A salt=((X1-X0)*X2)/X3=4.218mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=7.029mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 9:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 105 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 2727s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=2727s/51s=53.47;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)53.47 condition degree of numerical value, because E100 be more than 10 condition degree, take
White oil is added in residual oil 105.1g to be measured(Without inorganic salts)45g is diluted, and 30min is stirred using explosion-proof blender, by above-mentioned
A2 steps are tested, and the residual oil E100 after dilution is measured(100 DEG C of Engler viscosity)For 8.08 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 0.99g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 86.6%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
6.744mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 4.99mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;After b8, dilution
The salt content of residual oil is calculated as follows:A salt=((X1-X0)*X2)/X3=6.758mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=9.652mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Embodiment 10:A kind of residual oil salt content assay method that the present invention mentions, the test method carry out as follows:
A, the measurement of residual oil Engler viscosity to be measured:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
If sample containing water new calcining and cooling salt should be added, sodium sulphate or granular anhydrous calcium chloride carries out in filtered sample
It shakes, strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle true after standing sedimentation
Sky pump depressurizes 10min to remove), residual oil to be measured is heated to 109 DEG C after filtering, and 30min is stirred using explosion-proof blender;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Clean solvent oil carefully wash the inner pressurd vessel and its effuser of viscosimeter, then use air blow drying, the inaccurate wiping of inner pressurd vessel, only
Allow the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will add in advance
In heat to the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;In sample
When thermometer reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts
Stopper makes extra sample flow down, until pasta is just exposed in the tip of three spikes.If the sample of outflow is excessive,
Just mend that add sample full to the tip of spike dropwise, but in oil should not there are bubbles, after viscosimeter is plus lid, below tap hole
Place clean, dry receiving flask.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred and is tried using thermometer
Sample when the thermometer in sample reaches set point of temperature just, then keeps 5min (but without stirring), just lifts stopper rapidly,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time 3208s of sample,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter to use successively petroleum ether (or
Ether) 95% ethyl alcohol and distillation water washing, air blow drying is used in combination;Then the short-leg of viscosimeter is put into the hole of metal tripod,
It is fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using being washed successively with chromic acid in advance
The careful washed receiving flask of liquid, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;Until
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, again with mutually synthermal water mounted in the outer of viscosimeter
In container, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod adjusts the position of viscosimeter
It sets, the tip of three spikes in inner pressurd vessel is made to be in same level.Undried empty receiving flask is placed on inner pressurd vessel
Effuser below.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current outflow for not calculating water
Time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into effuser immediately
It is interior, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then empty receiving flask is placed on
It is inverted 1 ~ 2min on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask below effuser.Water in inner pressurd vessel
It will be sufficiently stirred with the liquid in outer container;First to stir water, then the lid for being inserted with thermometer is rotated around stopper
Heat insulation liquid is stirred with the blade mixer in outer container.When in two containers water and fluid temperature be equal to 20 DEG C
(temperature difference is no more than ± 0.2 DEG C in 6min) and inner pressurd vessel is adjusted to horizontality and (just reveals at the tip of three spikes
Go out the water surface) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly, starts simultaneously
Stopwatch.At this point, the case where observation water is flowed out from inner pressurd vessel, when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask,
Stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation result and its arithmetic
The difference of average value is not more than 0.5s, the average delivery time for just using this arithmetic mean of instantaneous value to be measured as first time.In addition, with
It also requires that and carries out another secondary parallel determination, and calculate the satisfactory average delivery time.If the mean flow of replication
The difference for going out the time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, at that time
Between be 51s, the water number of standard viscosimeter should be equal to 51 ± 1s.If water number does not allow for surveying using the instrument not in this range
Determine viscosity;
A4, residual oil Engler viscosity are calculated as follows:The condition degree of E100=T1/T2=3208s/51s=62.9;
In examination:E100-- residual oil Engler viscosity, condition degree;T1---- samples are flowed out in 100 DEG C of test temperature from viscosimeter
Time needed for 200mL, s;The water number of T2---- grace formula viscosimeters, s;
B, after dilution the salt content of residual oil measurement:
B1, residual oil E100 to be measured is measured(100 DEG C of Engler viscosity)62.9 condition degree of numerical value, because E100 be more than 10 condition degree, take
White oil is added in residual oil 102.5g to be measured(Without inorganic salts)43.9g is diluted, and 30min is stirred using explosion-proof blender, by upper
It states a2 steps to be tested, measures the residual oil E100 after dilution(100 DEG C of Engler viscosity)For 9.00 condition degree;
B2, the residual oil after dilution is heated to 70 DEG C, then stirs evenly sample, and quickly take 1.01g oil samples in centrifuge tube
In, 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water:3(Volume)Ratio mixed solution) alcohol -- aqueous solution, extract
Total amount, that is, extract, this amount must pipette accurately;
B3, centrifuge tube is put into 80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheat 1 point
Clock, then shaken 1 minute with flash mixer, it is then placed in centrifuge, is centrifuged 1 minute under 2000rpm rotating speeds, make grease point
From for apparent two-phase;B4, Microcoulomb instrument is opened, with fresh bath cleans electrolytic cell 3 times, 35ml electrolyte is added, from
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by left-to-right successively, adjust stirring
Sub- stability of rotation, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, adds salt content standard specimen to measure after baseline is steady flat
Equal conversion ratio is 86.1%;B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then is noted with a 0.25ml syringe
Enter air 2 times, then a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, rinse micro syringe and syringe needle 3 times, so
It uses micro syringe that 0.2ml samples are added to electrolytic cell afterwards, is repeated three times, measure the salt content that is averaged in residual oil after diluting
5.474mg/L;B6 and then selection and standard specimen similar in sample to be tested(A concentration of 5mg/L), reactionary slogan, anti-communist poster is carried out, the salt of standard specimen is measured
Content 5mg/L;B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content 0mg/L in blank;Slag after b8, dilution
The salt content of oil is calculated as follows:A salt=((X1-X0)*X2)/X3=5.474mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The detection of X1---- instruments does not correct the salt content of residual oil after dilution,
mg/L;X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1=7.818mg/L;
In examination:A salt -- the salt content of residual oil, mg/L after dilution;The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
A kind of residual oil salt content assay method that the present invention mentions, includes the following steps:
1, the measurement of residual oil Engler viscosity to be measured:
1.1 take residual oil sample 1000g to be measured, before measuring viscosity, have the metal of at least 576 eyelets to filter with each square centimeter
Net filtration sample, if sample containing water, should be added it is new calcine and cooling salt, sodium sulphate or granular anhydrous calcium chloride into
Row shakes, and strainer filtering is just used (when in sample containing not evanescent bubble, to allow to connect in sample bottle after standing sedimentation
Vacuum pump pressure 10min is removed), after filtering residual oil to be measured is heated to(100-110)DEG C, and stirred using explosion-proof blender
30min。
1.2 open instrument heating, open blender, wait for that instrument outer container fluid temperature reaches(99.8-100.2)DEG C when,
The inner pressurd vessel and its effuser of viscosimeter are carefully washed with the clean solvent oil of filtration, then use air blow drying, inner pressurd vessel inaccurate
Wiping, only allows the filter paper with edge of having one's hair trimmed to suck remaining drop, stopper is tightly clogged to the tap hole of viscosimeter, then will
It is previously heated in the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the tip of the necessary a little higher than spike of pasta of injection;Examination
When thermometer in sample reaches set point of temperature just, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly
It is micro- to lift stopper, so that extra sample is flowed down, until pasta is just exposed in the tip of three spikes.If the sample of outflow
Excessively, just mend that add sample full to the tip of spike dropwise, but should not there are bubbles to be flowed out after viscosimeter is plus lid in oil
Clean, dry receiving flask is placed below in hole.The lid for being inserted with thermometer is carefully rotated then around stopper, is stirred using thermometer
Sample is mixed, when the thermometer in sample reaches set point of temperature just, then 5min (but without stirring) is kept, just lifts wood rapidly
Plug, while stopwatch is started, when the sample in receiving flask is right up to the graticule of 200mL, the delivery time T1 of sample is read,
Constant to ± 0.2 DEG C of the fluid temperature of outer container is kept during experiment.
1.3 measure the water number of Engler viscometer simultaneously, and before measuring water number, the inner pressurd vessel of viscosimeter will use oil successively
95% ethyl alcohol of ether (or ether) and distillation water washing, are used in combination air blow drying;Then the short-leg of viscosimeter is put into metal tripod
In hole, fixed with fixing screws;At this point, clean, dry stopper is inserted into the upper hole of effuser;Using using chromium successively in advance
The careful washed receiving flask of pickle, water and distilled water, will be in (20 DEG C) injection viscosimeter inner pressurd vessels of the distilled water newly distilled;
Until the tip of three spikes in inner pressurd vessel is just exposed the surface;In addition, being mounted in viscosimeter with mutually synthermal water again
Outer container in, until being dipped into the enlarged of inner pressurd vessel.The adjusting screw of rotating metallic tripod, adjusts viscosimeter
Position makes the tip of three spikes in inner pressurd vessel be in same level.Undried empty receiving flask is placed on content
Below the effuser of device.Slightly lift stopper, the water in inner pressurd vessel is made all to be put into receiving flask, but the current stream for not calculating water
Go out the time.Water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water.Stopper is inserted into immediately and is flowed out
In pipe, the water in receiving flask is carefully injected in inner pressurd vessel along glass bar again, is sure not to splash out.Then, by empty receiving flask
It is placed on inner pressurd vessel and is inverted(1~2)Min makes the water in bottle flow completely out, then puts back to receiving flask below effuser.Inner pressurd vessel
In water and outer container in liquid will be sufficiently stirred;The lid for being inserted with thermometer is rotated around stopper to stir first
Then water stirs heat insulation liquid with the blade mixer being mounted in outer container.When the water and fluid temperature in two containers
It is adjusted to the horizontality (point of three spikes equal to 20 DEG C (in 6min temperature difference be no more than ± 0.2 DEG C) and inner pressurd vessel
Just expose the surface at end) when, lift stopper (should be able to stick automatically and keep the state lifted, not allow to extract stopper) rapidly,
Start stopwatch simultaneously.At this point, observation water the case where being flowed out from inner pressurd vessel, when concave meniscus lower edge to receiving flask 200mL rings
When shape graticule, stopwatch is stopped immediately.The time of distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times.If each time measures observation knot
The difference of fruit and its arithmetic mean of instantaneous value is not more than 0.5s, just uses this arithmetic mean of instantaneous value as when the average outflow measured for the first time
Between.In addition, carrying out another secondary parallel determination to also require that, and calculate the satisfactory average delivery time.If repeating to survey
The difference of fixed average delivery time is not more than 0.5s, just takes the arithmetic mean of instantaneous value of the two times result of this replication as instrument
The water number of water number, symbol T2, standard viscosimeter should be equal to(51±1)s.If water number does not allow for making not in this range
With the Instrument measuring viscosity.
The measurement of the salt content of residual oil after dilution:
2.1 measure residual oil E100 to be measured(100 DEG C of Engler viscosity)Numerical value E1 need to take to be measured when spending more than 10 conditions such as E1
White oil is added in residual oil 100-120g(Without inorganic salts)It is diluted, is uniformly mixed, by E100(100 DEG C of Engler viscosity)Control exists
(2-10)Between condition degree, and the quality m1 of residual oil and addition white oil when accurate recording dilution(Without inorganic salts)Quality m2.
2.2 are heated to the residual oil after dilution(50--70)DEG C, then sample is stirred evenly, and quickly takes(0.8-
1.2)In centrifuge tube 1.5ml dimethylbenzene is added, (95% ethyl alcohol presses 1 to 2.0ml with water in g oil samples:3(Volume)Ratio mixing it is molten
Liquid) alcohol -- aqueous solution, extract total amount, that is, extract, this amount must pipette accurately.
Centrifuge tube is put into 70~80 DEG C of water-baths and heats 1 minute by 2.3, is shaken 1 minute with flash mixer after taking-up,
It reheats 1 minute, then is shaken 1 minute with flash mixer, is then placed in centrifuge, in(2000-3000)Under rpm rotating speeds from
The heart(1-2)Minute, it is apparent two-phase to make water-oil separating.
2.4 open Microcoulomb instruments, and with fresh bath cleans electrolytic cell 2~3 times, 35ml electrolyte is added, from it is left extremely
Reference electrode, measuring electrode, electrolytic anode, electrolysis cathode are connected on titration cell binding post by the right side successively, are adjusted stirrer and are turned
It is dynamic steady, and pay attention to being protected from light, after connecting electrolytic cell, bias is mixed up, after baseline is steady plus salt standard specimen measures average conversion
It is advisable between 75%-100%.
One root long syringe needle is passed through oil reservoir to be inserted into centrifugation bottom of the tube by 2.5, then injects air 1 with a 0.25ml syringe
~2 times, a small amount of extracting solution is extracted in the oil discharge that will enter in syringe needle, micro syringe and syringe needle 2~3 times is rinsed, then with micro-
It measures syringe and 0.2ml samples is added to electrolytic cell, be repeated three times, measure the salt content X1 that is averaged in residual oil after diluting.
Then 2.6 select and standard specimen similar in sample to be tested(A concentration of X2), reactionary slogan, anti-communist poster is carried out, the salt content of standard specimen is measured
X3。
2.7 dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content X0 in blank.
3, points for attention
Before 3.1 measure grace formula viscosity every time, inner pressurd vessel and its outflow of viscosimeter are carefully washed with the clean solvent oil of filtration
Pipe, then uses air blow drying.The inaccurate wiping of inner pressurd vessel, only allows the filter paper with edge of having one's hair trimmed to suck remaining drop.
When 3.2 measurement grace formula viscosity, bubble, the tip of the necessary a little higher than spike of pasta of injection should not be generated in sample.
3.3 before measuring grace formula viscosity, first measures the water number of Engler viscometer, and the water number of standard viscosimeter should be equal to 51
± 1s, if water number does not allow for using the Instrument measuring viscosity not in this range.
When 3.4 measurement dilution residual oil salt content, if water-oil separating is unclear, heating -- mixing -- centrifugation step is repeated, if
Though grease detaches but water phase is unclear, this is not influenced as a result, can be analyzed as usual.
When 3.5 measurement dilution residual oil salt content, if sample sulfide content is excessively high, 1 drop 30%H need to be added2O2, to eliminate
Interference.
3.6 when measuring dilution residual oil salt content, repetition measurement once standard specimen again after determination sample, to determine the standard of instrument
True property and stationarity.
4, result calculates
(1) calculates 4.1 residual oil Engler viscosity as the following formula:
E100=T1/T2----------------------------(1)
In examination:E100-- residual oil Engler viscosity, condition degree;
T1---- samples flow out from viscosimeter the time needed for 200mL, s in 100 DEG C of test temperature;
The water number of T2---- grace formula viscosimeters, s;
(2) calculate the salt content of residual oil as the following formula after 4.2 dilutions:
A salt=((X1-X0)*X2)/X3---------------(2)
In examination:
A salt -- the salt content of residual oil, mg/L after dilution;
The detection of X1---- instruments does not correct the salt content of residual oil after dilution, mg/L;
X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;
The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L;
4.3 residual oil salt contents are as the following formula(3)It calculates:
A slags=A salt *(m1+m2)/m1----------------(3)
In examination:
The salt content of A slags -- residual oil, mg/L;
A salt -- the salt content of residual oil, mg/L after dilution;
The quality of residual oil, g when m1---- dilutes;
White oil is added in m2----(Without inorganic salts)Quality, g.
Subordinate list 1
The above is only the part preferred embodiment of the present invention, and any technical person familiar with the field is possibly also with upper
Equivalent technical solution is changed or be revised as to the technical solution for stating elaboration.Therefore, technical solution according to the present invention
Any simple modification carried out or substitute equivalents, belong to the greatest extent the scope of protection of present invention.
Claims (7)
1. a kind of residual oil salt content assay method, it is characterized in that including the following steps:It is equal by being stirred after residual oil heating and melting to be measured
It is even, the numerical value E1 of its 100 DEG C of Engler viscosity is measured, when being spent more than 10 conditions such as E1, needs addition white oil to be diluted, mixing is equal
It is even, by E100 DEG C of Engler viscosity control between 2-10 condition degree, with salt content in residual oil after alcohol-water mixture extracting dilution, use
Salt content in small-hole drilling or Potentiometric Determination residual oil,
The white oil uses the white oil without inorganic salts.
2. residual oil salt content assay method according to claim 1, it is characterized in that carrying out as follows:
A, the measurement of residual oil Engler viscosity to be measured:Residual oil to be measured is heated to 100-110 DEG C, and is stirred evenly;In test temperature
Time at 100 DEG C from viscosimeter needed for outflow 200mL, while the water number of Engler viscometer is measured, calculate 100 DEG C of slag
Oily Engler viscosity;
B, after dilution the salt content of residual oil measurement:The numerical value E1 for measuring 100 DEG C of Engler viscosity of residual oil to be measured, as E1 is more than 10
When part is spent, needs that white oil of the residual oil 100-120g additions without inorganic salts to be measured is taken to be diluted, be uniformly mixed, by 100 DEG C of grace
Family name's viscosity controls between 2-10 condition degree, and the quality m1 of residual oil and addition are free of the white oil of inorganic salts when accurate recording dilution
Quality m2;
C, residual oil salt content, mg/L=A salt *(m1+m2)/m1
In examination:
A salt -- the salt content of residual oil, mg/L after dilution;
The quality of residual oil, g when m1---- dilutes;
The quality of the white oil without inorganic salts, g is added in m2---.
3. residual oil salt content assay method according to claim 2, it is characterized in that:In step a, residual oil Engler viscosity to be measured
Measurement include the following steps:
A1, residual oil to be measured is heated to 100-110 DEG C, and stirred evenly;
A2, instrument heating is opened, opening blender first will be wooden when instrument outer container fluid temperature reaches 99.8-100.2 DEG C
Plug tightly clogs the tap hole of viscosimeter, then will be previously heated in the residual oil injection inner pressurd vessel of a little higher than set point of temperature, note
The pasta entered is higher than the tip of spike;When thermometer in sample reaches set point of temperature, then 5min is kept, then lifts stopper,
Stopwatch is started simultaneously, when the sample in receiving flask is right up to the graticule of 200mL, reads the delivery time T1 of sample;
A3 while the water number for measuring Engler viscometer are that distilled water flows out the time needed for 200mL at 20 DEG C from viscosimeter
T2;
A4, residual oil Engler viscosity are calculated as follows:
E100=T1/T2
In examination:
E100-- residual oil Engler viscosity, condition degree;
T1---- samples flow out from viscosimeter the time needed for 200mL, s in 100 DEG C of test temperature;
The water number of T2---- grace formula viscosimeters, s.
4. residual oil salt content assay method according to claim 2, it is characterized in that:The salt content of residual oil after the dilution
It measures, includes the following steps:
B1, the numerical value E1 for measuring 100 DEG C of Engler viscosity of residual oil to be measured, when spending more than 10 conditions such as E1, need to take residual oil to be measured
100-120g is added the white oil without inorganic salts and is diluted, and is uniformly mixed, by 100 DEG C of Engler viscosity controls in 2-10 condition degree
Between, and the quality m1 of residual oil and addition are free of the quality m2 of the white oil of inorganic salts when accurate recording dilution;
B2, the residual oil after dilution is heated to 50--70 DEG C, then stirs evenly sample, and quickly take 0.8-1.2g oil samples in
In centrifuge tube, 1.5ml dimethylbenzene, 2.0ml alcohol-aqueous solution is added;
B3, centrifuge tube is put into 70~80 DEG C of water-baths and is heated 1 minute, shaken 1 minute with flash mixer after taking-up, reheated
1 minute, then shaken 1 minute with flash mixer, it is then placed in centrifuge, 1~2 is centrifuged under 2000~3000rpm rotating speeds
Minute, it is apparent two-phase to make water-oil separating;
B4, Microcoulomb instrument is opened, after connecting electrolytic cell, mixes up bias, after baseline is steady plus salt standard specimen measures average transformation
Rate is advisable between 75%-100%;
B5, a root long syringe needle is passed through oil reservoir be inserted into centrifugation bottom of the tube, then air is injected 1~2 time with a 0.25ml syringe,
The oil discharge that will enter in syringe needle, then extracts a small amount of extracting solution, micro syringe and syringe needle 2~3 times is rinsed, then with micro
0.2ml samples are added to electrolytic cell in syringe, are repeated three times, and measure the salt content X1 that is averaged in residual oil after diluting;
B6 and then selection and standard specimen similar in sample to be tested, a concentration of X2 carry out reactionary slogan, anti-communist poster, measure the salt content X3 of standard specimen;
B7, dimethylbenzene, alcohol -- aqueous solution carry out blank assay, record salt content X0 in blank;
The salt content of residual oil is calculated as follows after b8, dilution:
A salt=((X1-X0)*X2)/X3
In examination:
A salt -- the salt content of residual oil, mg/L after dilution;
The detection of X1---- instruments does not correct the salt content of residual oil after dilution, mg/L;
X2---- reactionary slogan, anti-communist poster standard specimen salt contents, mg/L;
The detection of X3---- instruments does not correct reactionary slogan, anti-communist poster standard specimen salt content, mg/L;
Salt content in X0---- blank, mg/L.
5. residual oil salt content assay method according to claim 2, it is characterized in that:In the residual oil excessively high to sulfide content
When salt content measures, 1 drop 30%H is added2O2, to eliminate interference, if 30% H is added2O2, take 2ml water samples in centrifugation in b3 steps
Guan Zhong is heated 1 minute in 70 DEG C of water-baths, and 1 30% H of drop is then added2O2, wait for that water sample is cooled to room temperature progress after being vigorously mixed
Analysis.
6. residual oil salt content assay method according to claim 2, it is characterized in that:When salt content measures, after processing
Acetic acid electrolyte of the sample injection containing silver ion in, chlorion in sample reacts with silver ion:
Cl-+Ag+→ AgCl↓
The silver ion for reacting consumption gives birth to supplement by generation electrode electricity, by measuring the electricity of the raw silver ion consumption of electricity, according to farad
Law can acquire salt content.
7. residual oil salt content assay method according to claim 2, it is characterized in that:In step a, residual oil Engler viscosity to be measured
Measurement comprise the following specific steps that:
A1, residual oil sample 1000g to be measured is taken, before measuring viscosity, there is the metal screen of at least 576 eyelets with each square centimeter
Filtered sample is added new calcining and cooling salt, sodium sulphate or granular anhydrous calcium chloride is shaken if sample containing water
It is dynamic, strainer filtering is just used after standing sedimentation, residual oil to be measured is heated to 105 DEG C after filtering, and stir using explosion-proof blender
Mix 30min;
A2, instrument heating is opened, blender is opened, when instrument outer container fluid temperature reaches 99.8-100.2 DEG C, with filtration
Cleaning solvent oil wash viscosimeter inner pressurd vessel and its effuser, then use air blow drying, inner pressurd vessel is not required to wipe, and only allows
Remaining drop is sucked with the filter paper at edge of having one's hair trimmed, stopper is tightly clogged to the tap hole of viscosimeter, then will be previously heated to
In the residual oil injection inner pressurd vessel of a little higher than set point of temperature, the pasta of injection is higher than the tip of spike;Thermometer in sample up to
When to set point of temperature, then 5min is kept, specimen temperature answers constant to ± 0.2 DEG C in inner pressurd vessel, slightly lifts stopper, and it is extra to make
Sample flows down, until pasta is just exposed in the tip of three spikes;If the sample of outflow is excessive, just mends dropwise and add sample
It not add after covering, be placed below in tap hole clean, dry there are bubble, viscosimeter completely to the tip of spike, but in oil
Receiving flask;The lid for being inserted with thermometer is carefully rotated then around stopper, and sample, the temperature in sample are stirred using thermometer
Meter is just when reaching set point of temperature, then keeps 5min, but without stirring, just lifts stopper rapidly, while starting stopwatch, when connecing
When sample in by bottle is right up to the graticule of 200mL, the delivery time 4946s of sample is read, to be kept during the test
Constant to ± 0.2 DEG C of the fluid temperature of outer container;
A3 while the water number for measuring Engler viscometer, before measuring water number, the inner pressurd vessel of viscosimeter will use petroleum ether successively, and 95%
Ethyl alcohol and distillation water washing, are used in combination air blow drying;Then viscosimeter metal tripod is put into fix;At this point, by clean, dry
Stopper be inserted into effuser upper hole in;Using using chromic acid lotion successively in advance, the careful washed receiving flask of water and distilled water,
The distilled water newly distilled is injected in viscosimeter inner pressurd vessel;Until inner pressurd vessel in three spikes tip just exposed the surface for
Only;In addition, again with mutually synthermal water in the outer container of viscosimeter, until being dipped into the enlarged of inner pressurd vessel;It adjusts
The position of whole viscosimeter makes the tip of three spikes in inner pressurd vessel be in same level;Undried sky is received
Bottle is placed on the effuser of inner pressurd vessel in the following, slightly lifting stopper, and the water in inner pressurd vessel is made all to be put into receiving flask, but specifically not
The delivery time for calculating water, water is filled in effuser at this time, and the bottom end of effuser is made to poise a big drop of water, it immediately will be wooden
Plug is inserted into effuser, is again carefully injected in inner pressurd vessel the water in receiving flask along glass bar, is sure not to splash out, then,
Empty receiving flask is placed on 1 ~ 2min of inversion on inner pressurd vessel, so that the water in bottle is flowed completely out, then puts back to receiving flask under effuser
Face, the liquid in water and outer container in inner pressurd vessel will be sufficiently stirred;The lid for being inserted with thermometer is rotated around stopper first
To stir water, then be mounted on outer container in blade mixer stir heat insulation liquid, when in two containers water and
Fluid temperature is equal to 20 DEG C, and when inner pressurd vessel is adjusted to horizontality, lifts stopper rapidly, while starting stopwatch, at this point, seeing
The case where Cha Shui is flowed out from inner pressurd vessel stops the second immediately when the 200mL ring-type graticules of the lower edge of concave meniscus to receiving flask
The time of table, distilled water outflow 200mL wants METHOD FOR CONTINUOUS DETERMINATION four times, if each difference for measuring observation result and its arithmetic mean of instantaneous value
Number be not more than 0.5s, just use this arithmetic mean of instantaneous value as the first time measurement the average delivery time, in addition, with also require that into
Another secondary parallel determination of row, and the satisfactory average delivery time is calculated, if the difference of the average delivery time of replication
No more than 0.5s, just take the arithmetic mean of instantaneous value of the two times result of this replication as the water number of instrument, time 51s, mark
The water number of quasi- viscosimeter should be equal to 51 ± 1s, if water number does not allow for using the Instrument measuring viscosity not in this range;
A4, residual oil Engler viscosity are calculated as follows:
E100=T1/T2
In examination:
E100-- residual oil Engler viscosity, condition degree;
T1---- samples flow out from viscosimeter the time needed for 200mL, s in 100 DEG C of test temperature;
The water number of T2---- grace formula viscosimeters, s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109613133A (en) * | 2018-12-19 | 2019-04-12 | 东营联合石化有限责任公司 | Each fraction of residual oil can extracting rate measuring method in a kind of crude oil |
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