CN102645526A - Device for determining water content in petroleum products by using distillation method and method for device - Google Patents
Device for determining water content in petroleum products by using distillation method and method for device Download PDFInfo
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- CN102645526A CN102645526A CN2012101445677A CN201210144567A CN102645526A CN 102645526 A CN102645526 A CN 102645526A CN 2012101445677 A CN2012101445677 A CN 2012101445677A CN 201210144567 A CN201210144567 A CN 201210144567A CN 102645526 A CN102645526 A CN 102645526A
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Abstract
The invention discloses a device for determining water content in petroleum products by a distillation method and a method for the device. The device comprises a distillation flask, a receiver, a condenser pipe, a heater, a sprayer and an ultrasonic cleaner, wherein the ultrasonic cleaner is located on a work bench beside the receiver, and tap water is contained in the ultrasonic cleaner. The method comprises the following steps of performing distillation and condensation according to the prior standard; taking down the receiver which is cooled to the room temperature, placing the receiver into the ultrasonic cleaner, and performing ultrasonic processing for 5-20 seconds at the frequency of 30-60 khz at the temperature from 15 DEG C to 35 DEG C; and reading the water volume in the receiver according to the prior standard. According to the device for determining the water content in the petroleum products by using the distillation method and the method for the device, the ultrasonic cleaner is used for processing water drops on the side wall of the receiver, and simultaneously, minor water drops in a solvent are enabled to effectively fall back to the water layer, so that personal errors caused by different testing persons who process the water drops on the receiver are avoided, and errors due to the usage of different scrapers among different standards are avoided.
Description
Technical field
The present invention relates to a kind of technology of measuring liquid water content in the petroleum products, relate in particular to the devices and methods therefor that a kind of way of distillation is measured liquid water content in the petroleum products.
Background technology
Oil is the important strategic resource, is concerning the economic security of country.Along with rapid development of economy, domestic petroleum and products thereof consumption significantly increases, and become net import of oil state from China in 1993 and begin, about 1,000 ten thousand tons of import volume average annual growths, import volume was near 200,000,000 tons in 2011.But aspect the check at Imported oil and products thereof--weight and the quality examination, Chinese Industrial Standards (CIS) and other countries' standard and international standard have many difference.The link that relates to the check evaluation in the trade in oil process mainly comprises sampling, quality restriction and three links of metering evaluation, and three links all possibly produce significant impact to final trade result.Wherein, liquid water content directly influences international petroleum trade charging in the petroleum products.
1, the test stone brief introduction of water cut in the petroleum products
Liquid water content generally is present in the total amount of all phase water such as free water in the petroleum products, emulsified water, dissolving water in the petroleum products.With quality or volume percentage note, represent with percentage usually.The liquid water content method of testing is divided into the way of distillation, centrifuge method, karl Fischer method and electricity from principle and takes off four types of methods in the petroleum products, but the most frequently used be the way of distillation.
The distillation ratio juris is: a certain amount of sample mixes with anhydrous solvent, under situation about refluxing, heats, and solvent is separated in receiver with water continuously, and water is deposited in the scale part of receiver, and solvent then returns distiller.Way of distillation characteristics are: measurement range is bigger, and all available way of distillation of the water cut more than 0.1% detects.Easy and simple to handle, cost is low, and is safer, for domestic sectors generally adopts, is the main method of water cut test in the China's oil product.
2, domestic and international standard present situation
(1) Russian standard
GOST 2477-65 oil and petroleum products liquid water content determination method (way of distillation).
GOST R ISO 3734-2009 crude oil and fuel W/O and sediment determination method (centrifuge method).
(2) Chinese Industrial Standards (CIS)
GB/T 260-77 petroleum products aquametry (way of distillation).
The mensuration (electricity takes off method) of SY/T5402 Water Content in Oil amount.
(3) international standard
Water in ISO 3734 crude oil and the fuel oil and sediment determination method (centrifuge method).
3, the way of distillation test method standard of petroleum products liquid water content comparison
The main method of petroleum products water cut test generally adopts the way of distillation at home and abroad.Russia national standard GOST P51858-2002 regulation petroleum products liquid water content assay method is GOST 2477-65 " determination method of oil and petroleum products liquid water content ", and the method is the way of distillation.Similar with it standard has CNS GB/T 260-77 " petroleum products aquametry (way of distillation) " etc.
These standard methods all are the way of distillations; Principle is basic identical; All be the mode through refluxing, with sample and water-immiscible solvent Hybrid Heating, the water in the sample is by distillation simultaneously; Condensed solvent separates in receiver with water, calculates the content of water in crude oil or the petroleum products according to the amount of water in the receiver.
The main difference of standard is:
(1) scope of application: GOST 2477-65 is applicable to liquid petroleum product, railway grease, paraffin, ceresine, wax work, pitch and crude oil; GB/T 260-77 is applicable to petroleum products.
(2) solvent: GOST 2477-65 regulation solvent is 80～120 ℃ of straight-run clear gasolines, and its arene content is less than 3%; GB/T 260-77 regulation solvent is straight-run gasoline or an industrial solvent more than 80 ℃.
(3) instrument: GOST2477-65 is identical with instrument among the GB/T260-77.
The test period of (4) test period: GOST2477-65 regulation is for being no more than 1 hour; The return time of GB/T260-77 regulation is no more than 1 hour.
4, the defective of the way of distillation test method of petroleum products liquid water content
Measure the way of distillation of liquid water content in the petroleum products, on the sidewall of glass receiver, be stained with minor amount of water, cause liquid water content on the low side.The GOST2477-65 regulation, the minor amount of water that is stained with on the sidewall of glass receiver adopts the metal scraping to scrape in the backwater layer; The GB/T260-77 regulation, the minor amount of water that is stained with on the sidewall of glass receiver, an end that adopts tinsel or thin glass bar to have rubber or plastic cap scrapes in the backwater layer.There is defective in the method that employing scraping etc. scrapes in the backwater layer; The personal error that mainly is different testing crew is big; And GOST2477 and GB/T260-77 are because scraping different; Error is at 0.03%-0.05%, and the trade settlement loss that annual several ten million tons of petroleum productss are imported and exported is worth at several hundred million yuans.
Summary of the invention
For overcoming the problems referred to above that prior art exists, the objective of the invention is to propose a kind ofly can avoid manual work to scrape the devices and methods therefor that minor amount of water causes personal error, the way of distillation that improves the liquid water content accuracy of measurement is measured liquid water content in the petroleum products.
Technical solution of the present invention is achieved in that
A kind of way of distillation is measured the device of liquid water content in the petroleum products, comprises distilling flask, receiver, condenser pipe, well heater and sprayer, and taper ground A is arranged at described condenser pipe bottom; Condenser pipe connects receiver through taper ground A; Taper ground B is arranged at the receiver bottom, and receiver is connected with distilling flask through taper ground B, the solvent-laden petroleum products sample of the inner splendid attire of distilling flask; The having heaters in the distilling flask bottom, the bottom of said receiver are tubule and scale are arranged; Described sprayer is used at still-process, with the water droplet on the condenser pipe sidewall, blows off in receiver; Described device also comprises ultrasonic cleaner; Described ultrasonic cleaner is positioned on the worktable, tap water is equipped with in its inside.
A kind of way of distillation is measured the method for the device of liquid water content in the petroleum products, comprises the steps:
A, connect distilling flask, receiver, condenser pipe, well heater and sprayer by prior standard;
B, distill and condensation by prior standard;
After C, distillation finish, take off the receiver that is cooled to room temperature, receiver is put into ultrasonic cleaner, carry out sonicated according to the condition of time 5-20 second, frequency 30-60khz and temperature 15-35 ℃;
D, read the volume of water in the receiver by prior standard.
Prior standard of the present invention comprises GOST 2477-65 " oil and petroleum products liquid water content determination method (way of distillation) " or GB/T260-77 " petroleum products aquametry (way of distillation) ".
Compared with prior art, advantage of the present invention mainly shows:
1, because the present invention adopts ultrasonic unit to handle the water droplet on the receiver, avoided different tests personnel to handle the personal error of water droplet on the receiver.
2, because the present invention adopts ultrasonic unit to substitute scraping of the prior art, the error of having avoided between various criterion the method for the different scrapings of employing to cause.
3, because the present invention adopts ultrasonic unit to substitute scraping of the prior art, the micro-water droplet in the solvent is effectively fallen back in the water layer.
4, the present invention has good stable property and reappearance, and accuracy of detection is high.
5, the present invention can accurately measure liquid water content in the petroleum products, thus standard trade both sides' dispute.
Description of drawings
Drawings attached 1 width of cloth of the present invention, wherein:
Fig. 1 is a device synoptic diagram of the present invention.
Among the figure: 1, condenser pipe, 2, taper ground A, 3, receiver, 4, taper ground B, 5, distilling flask, 6, solvent-laden petroleum products sample, 7, well heater, 8, ultrasonic cleaner, 9, tap water, 10, solvent.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.As shown in Figure 1; A kind of way of distillation is measured the device of liquid water content in the petroleum products, comprises distilling flask 5, receiver 3, condenser pipe 1, well heater 7 and sprayer, and taper ground A2 is arranged at described condenser pipe 1 bottom; Condenser pipe 1 connects receiver 3 through taper ground A2; Taper ground B4 is arranged at receiver 3 bottoms, and receiver 3 is connected with distilling flask 5 through taper ground B4, the solvent-laden petroleum products sample 6 of distilling flask 5 inner splendid attires; At distilling flask 5 bottom having heaters 7, the bottom of said receiver 3 is tubule and scale is arranged; Described sprayer is used at still-process, with the water droplet on condenser pipe 1 sidewall, blows off in receiver 3; Described device also comprises ultrasonic cleaner 8; Described ultrasonic cleaner 8 is positioned on the worktable, tap water 9 is equipped with in its inside.Said distilling flask is the 500mL round-bottomed flask.
The Device Testing process that a kind of way of distillation is measured liquid water content in the petroleum products comprises:
With distilling flask 5 heating, petroleum products sample and solvent 10 are seethed with excitement; Distillation time is no more than 1 hour; Circulating water temperature in the condenser pipe 1 is at 20-25 ℃; , blow off in receiver 3 water droplet on condenser pipe 1 sidewall with sprayer; Receiver 3 bottoms are water layer, and top is solvent layer, sticking micro-water droplet on the wall of receiver 3; Receiver 3 is put into ultrasonic cleaner 8 carry out sonicated; During mensuration, receiver 3 bottoms are tubule and scale are arranged that liquid water content is read through scale mark.
Below in conjunction with instance the present invention is described further.
Press the GB/T260-77 regulation; Used solvent distillation 10 is an industrial solvent; Accurately take by weighing a certain amount of petroleum products sample with balance and add the 500mL round-bottomed flask; With graduated cylinder get an amount of paint industry with solvent oil or more than 80 ℃ straight-run gasoline add the 500mL round-bottomed flask, regulate the heating voltage of well heater 7, make the speed that distillate drips with per second 2-4 drip into receiver 3; , blow off in receiver 3 water droplet on condenser pipe 1 sidewall with sprayer; But in condenser pipe 1, have no the volume of water in water breakthrough and the receiver 3 at least 5 minutes, to remain constant, stop distillation; Receiver 3 is put into ultrasonic cleaner 8 carry out sonicated; During mensuration, receiver 3 bottoms are tubule and scale are arranged that liquid water content is read through scale mark.
Experimental example 1: with certain inlet opening fuel oil is laboratory sample; The fuel oil sample that accurately takes by weighing 100 grams with balance adds the 500mL round-bottomed flask; The paint industry of getting 100mL with graduated cylinder adds the 500mL round-bottomed flask with solvent oil; Regulate the heating voltage of electrical heating cover, make the speed that distillate drips with per second 2-4 drip into receiver 3; , blow off in receiver 3 water droplet on condenser pipe 1 sidewall with sprayer; But in condenser pipe 1, have no the volume of water in water breakthrough and the receiver 3 at least 5 minutes, to remain constant, stop heating.When receiver 3 is cooled to room temperature, put into ultrasonic cleaner 8, carry out sonicated for 25 ℃ according to 10 seconds time, frequency 40khz, temperature; During mensuration, receiver 3 bottoms are tubule and scale are arranged that liquid water content is read through scale mark.Mensuration result of the present invention is 2.80% (m/m), and the mensuration result of GB/T260-77 is 2.60% (m/m).
Experimental example 2: with domestic certain fuel oil is laboratory sample; The fuel oil sample that accurately takes by weighing 100 grams with balance adds the 500mL round-bottomed flask; The straight-run gasoline more than 80 ℃ of getting 100mL with graduated cylinder adds the 500mL round-bottomed flask; Regulate the heating voltage of electrical heating cover, make the speed that distillate drips with per second 2-4 drip into receiver 3; , blow off in receiver 3 water droplet on condenser pipe 1 sidewall with sprayer; But in condenser pipe 1, have no the volume of water in water breakthrough and the receiver 3 at least 5 minutes, to remain constant, stop heating.When receiver 3 is cooled to room temperature, put into ultrasonic cleaner 8, carry out sonicated for 30 ℃ according to 10 seconds time, frequency 40khz, temperature; During mensuration, receiver 3 bottoms are tubule and scale are arranged that liquid water content is through the scale mark reading.Mensuration result of the present invention is 5.60% (m/m), and the mensuration result of GB/T260-77 is 5.40% (m/m).
More than two Test Example show that liquid water content measured value of the present invention is more near actual value, water and the water in the solvent 10 on receiver 3 walls flow in the water layer more fully, it is more accurate to measure the result.
Claims (3)
1. the way of distillation is measured the device of liquid water content in the petroleum products; Comprise distilling flask (5), receiver (3), condenser pipe (1), well heater (7) and sprayer; Taper ground A (2) is arranged at described condenser pipe (1) bottom, and condenser pipe (1) connects receiver (3) through taper ground A (2), and taper ground B (4) is arranged at receiver (3) bottom; Receiver (3) is connected with distilling flask (5) through taper ground B (4); The solvent-laden petroleum products sample of the inner splendid attire of distilling flask (5) (6), at distilling flask (5) bottom having heaters (7), the bottom of said receiver (3) is tubule and scale is arranged; Described sprayer is used at still-process, with the water droplet on condenser pipe (1) sidewall, blows off in receiver (3); It is characterized in that: described device also comprises ultrasonic cleaner (8); Described ultrasonic cleaner (8) is positioned on the worktable, tap water (9) is equipped with in its inside.
2. the way of distillation is measured the method for the device of liquid water content in the petroleum products, it is characterized in that: comprise the steps:
A, connect distilling flask (5), receiver (3), condenser pipe (1), well heater (7) and sprayer by prior standard;
B, distill and condensation by prior standard;
After C, distillation finish, take off the receiver (3) that is cooled to room temperature, receiver (3) is put into ultrasonic cleaner (8), carry out sonicated according to the condition of time 5-20 second, frequency 30-60khz and temperature 15-35 ℃;
D, read the volume of water in the receiver (3) by prior standard.
3. a kind of way of distillation according to claim 2 is measured the method for the device of liquid water content in the petroleum products, and it is characterized in that: described prior standard comprises GOST 2477-65 " oil and petroleum products liquid water content determination method (way of distillation) " or GB/T260-77 " petroleum products aquametry (way of distillation) ".
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| CN201210144567.7A CN102645526B (en) | 2012-05-10 | 2012-05-10 | Device for determining water content in petroleum products by using distillation method and method for device |
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| CN201210144567.7A CN102645526B (en) | 2012-05-10 | 2012-05-10 | Device for determining water content in petroleum products by using distillation method and method for device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104076130A (en) * | 2014-07-11 | 2014-10-01 | 中国人民解放军空军勤务学院 | Method for quickly detecting content of insoluble water in jet fuel |
| CN108918324A (en) * | 2018-06-04 | 2018-11-30 | 中国石油化工股份有限公司 | The separator and method for quantitatively determining of oil, Free water, irreducible water in rock |
| CN115561435A (en) * | 2022-10-08 | 2023-01-03 | 南京市中环利安工程技术有限公司 | Lubricating oil gas phase detection device and method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104076130A (en) * | 2014-07-11 | 2014-10-01 | 中国人民解放军空军勤务学院 | Method for quickly detecting content of insoluble water in jet fuel |
| CN108918324A (en) * | 2018-06-04 | 2018-11-30 | 中国石油化工股份有限公司 | The separator and method for quantitatively determining of oil, Free water, irreducible water in rock |
| CN108918324B (en) * | 2018-06-04 | 2024-04-12 | 中国石油化工股份有限公司 | Separation device for oil, free water and bound water in rock and quantitative determination method |
| CN115561435A (en) * | 2022-10-08 | 2023-01-03 | 南京市中环利安工程技术有限公司 | Lubricating oil gas phase detection device and method thereof |
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