Method for determining the limiting filterability temperature on a cold filter. Method for determining the limiting filterability temperature on a cold filter Fig. 8

GOST 22254-92

Group B19

STATE STANDARD OF THE UNION OF THE SSR

FUEL DIESEL

Method for determining the limiting filterability temperature on a cold filter

diesel fuels. Cold filter method for determination of lowest filtering temperature

OKSTU 0251

Introduction date 1993-01-01

INFORMATION DATA

1. PREPARED AND INTRODUCED by the All-Union Research Institute for Oil Refining (VNII NP)

2. APPROVED AND INTRODUCED BY Decree of the Committee for Standardization and Metrology of the USSR of 03.02.92 N 101

During the development of this standard, some provisions of the European standard EN-116 "Standard method for determining the limiting filterability temperature of cold filter fuels" were used.

3. REPLACE GOST 22254-76

4. REFERENCE REGULATIONS AND TECHNICAL DOCUMENTS

1. PURPOSE

1. PURPOSE

This International Standard specifies a method for the determination of the cold filter plugging point of diesel and domestic heating oils intended for the national economy and for export.

Additions reflecting the needs of the national economy are in italics.

2. APPLICATION

The method applies to diesel fuels without additives and with additives, as well as fuels used in domestic heating systems.

3. DEFINITION

Filterability limit temperature (cold filter) - the highest temperature at which a given volume of fuel does not flow through a standardized filter unit for a certain time, during cooling under standardized conditions.

4. ESSENCE OF THE METHOD

The method consists in gradually cooling the test fuel at intervals of 1 °C and draining it through a wire filter mesh at a vacuum of 1961 Pa (200 mm w.c.).

The determination is carried out up to a temperature at which the paraffin crystals released from the solution onto the filter cause the flow to stop or slow down to such an extent that the pipette filling time exceeds 60 s, or the fuel does not drain completely back into the measuring vessel.

5. MATERIALS AND REAGENTS

5.1. White spirit, boiling in the range of 60-80 ° C.

5.2. Acetone.

5.3. The filter paper is non-fibrous.

Solvents: nefras C 50/170 to GOST 8505 or petroleum ether according to TU 6-021244;

Acetone by GOST 2603 ;

Paper filters "White tape".

6. EQUIPMENT

For testing, equipment according to drawing 1 is used, which includes:

6.1. Measuring vessel (5) - cylindrical, flat-bottomed transparent glass, inner diameter (31.5±0.5) mm, wall thickness (1.25±0.25) mm and height (120±5) mm, with restrictive ring a mark at a height corresponding to a volume of 45 cm.

Damn.1. Full set of equipment

Full set of equipment

1 - cooling bath; 2 - insulating ring; 3 - gasket; 4 - filter; 5 - measuring vessel;
6 - gasket; 7 - casing; 8 - supporting ring; 9 - cork; 10 - pipette; 11 - gauge
label (20 cm); 12 - three-way stopcock; 13 - U-shaped manometer; 14 - water;
15 - connection with the atmosphere; 16 - connection with a vacuum pump; 17 - glass bottle
(buffer capacity); 18 - water level

Measuring vessels of the required dimensions can be selected from vessels that meet the requirements of the GOST 20287 method.

6.2. Metal casing (Fig. 2) - brass, cylindrical, waterproof, flat-bottomed with an inner diameter of (45 ± 0.25) mm, an outer diameter of (48 ± 0.25) mm and a height of 115 mm. Used as a water bath.

Damn.2. Brass casing

Brass casing

1 - silver solder

6.3. Insulating ring (Fig. 3) - made of oil-resistant material, which is placed on the bottom of the casing (clause 6.2) to isolate the measuring vessel from the bottom. It must fit exactly to the casing and must be (6) mm thick.

Damn.3. Insulating ring and gaskets

Insulating ring and gaskets

1 - insulating ring; 2 - gaskets; 3a - stainless steel wires with a diameter of 2 mm

6.4. Two gaskets (3 and 6) 5 mm thick, made of oil-resistant material. Gaskets must fit snugly into the measuring vessel and loosely into the casing. The use of partial rings, each with a radial gap of 2 mm, allows the gaskets to be adapted to changes in the diameter of the measuring vessel. Gaskets and insulating ring can be made in one piece (see drawing 3).

6.5. A support ring (fig. 4) made of oil-resistant material to secure the casing (item 6.2) in a stable vertical position in the cooling bath, as well as to keep the plug (item 6.6) in a centered position. The ring can be modified to fit in a cooling bath.

Damn.4. support ring

support ring

Damn.4

6.6. Stopper (Fig. 5) made of oil-resistant material, fitted to the measuring vessel and support ring. The stopper must have three openings: for a pipette (item 6.7), a thermometer (item 6.8) and an outlet to the atmosphere. If a thermometer with wider temperature limits is used, the top of the stopper may have a cut-out slot which allows the temperature to be read on the thermometer (6.8) down to minus 30 °C. A pointer should be attached to the top surface of the plug for the appropriate placement of the thermometer in relation to the bottom of the measuring vessel. A spring wire clamp must be used to hold the thermometer in the correct position.

Damn.5. Cork

Cork

1 - a slot that allows you to read the temperature down to minus 30 ° C; 2 - connection with the atmosphere;
3 - stainless steel clamp for fixing the thermometer

6.7. Pipette with filter

6.7.1. A pipette (Fig. 6) made of transparent glass with a calibration mark at a height of (149 ± 0.5) mm from the base of the pipette, corresponding to a volume of (20.0 ± 0.2) cm. The pipette is connected to the filter.

Damn.6. Pipette

Pipette

1 - calibration mark.

6.7.2. The filter (Fig. 7) consists of the following parts:

a brass body with a threaded hole in which a filtration mesh is placed in a mandrel. The hole must be fitted with a gasket made of oil-resistant plastic. Inner diameter of the central tube (4.0±0.1) mm;

brass nut to connect the top of the filter housing to the bottom of the pipette to ensure a tight connection. An example of a correct connection is shown in Fig. 7;

filter mesh 15 mm in diameter, made of bronze or stainless steel wire, with a nominal opening size of 45 µm. The nominal diameter of the wire shall be 32 µm and the tolerance of individual mesh dimensions shall be as follows:

Each cell must not exceed the nominal size by more than 22 µm.

The average cell size should not exceed the nominal size by ±3.1 µm.

Damn.7. Filter

Filter

1 - knurling;

2 - pipette tube; 3 - brass nut; 4 - gasket made of oil-resistant plastic, annular,
diameter 5.28x1.78; 5 - brass body; 6 - gasket made of oil-resistant plastic, annular,
diameter 12.42x1.78; 7 - filter mesh mandrel; 8 - brass cylinder with external thread

No more than 6% of the cells may exceed the nominal size by more than 13 microns;

a brass mandrel (Fig. 8), in which the filter mesh (clause 6.7.2) is clamped with a reinforcing ring squeezed into the holder. The diameter of the working part of the grid should be (12) mm;

Damn.8. Filter mesh mandrel

Filter mesh mandrel

1 - mandrel body; 2 - reinforcing ring: 3 - filtration mesh

a brass cylinder with an external thread, which can be screwed into the body hole (p. 6.7.2) to pressurize the mesh mandrel (p. 6.7.2) through the gasket (p. 6.7.2). At the bottom there should be four grooves to ensure that the sample flows into the filtration apparatus.

6.8. Thermometers with measurement limits from minus 30 to plus 50 °С - to determine the limiting filterability temperature up to minus 30 °С, from minus 80 to plus 20 °С - to determine the limiting filterability temperature below minus 30 °С,

thermometer for a cooling bath with temperature measurement limits from minus 80 to plus 20 °C.

Use thermometers that meet the requirements given in the appendix.

Note. Suitable thermometers for testing are IP, IC and 2C or ASTM 5C and 6C.

6.9. Cooling bath of any type, shaped and sized to accommodate the enclosure (6.2) in a stable vertical position to the required depth. The bath must be equipped with a lid with holes to strengthen the supporting ring with a casing and a thermometer (clause 6.8).

The casing may be firmly attached to the cover.

The temperature of the cooling bath must be maintained at the required level using a refrigerator or using an appropriate cooling mixture (Section 6).

For different filterability limit temperatures, the cooling bath temperatures given in Table 1 must be maintained. These are achieved either by using separate cooling baths or by adjusting the condenser. The use of a refrigerator makes it possible to quickly change the temperature of the bath.

If several samples to be analyzed are placed in one large cooling bath, the distance between them must be at least 50 mm.

6.10. Stopcock glass, three-way, inclined, hole diameter 3 mm.

6.11. Vacuum pump or water pump of sufficient capacity to provide a flow rate of 3 to 4 dm/h in the vacuum regulator (6.12) during the test.

6.12. Vacuum regulator (17) (fig. 1) - a glass bottle 350-400 mm high, with a capacity of 5 dm3, filled 3/4 with water, sealed with a stopper with three holes for glass tubes. The two tubes must be short and must not be submerged in water. The third tube with an internal diameter of about (6 ± 1) mm should be long enough so that one end of it is immersed in water by 200 mm, and the other protrudes above the stopper.

The depth of the immersed part must be set in such a way as to obtain a pressure drop across the pressure gauge containing water of exactly 200 mm of water.

The installation is shown in Fig.1.

6.13. Stopwatch with an error of 1.2

6.14. Semi-automatic apparatus for determining the limiting filterability temperature of PAF diesel fuels according to TU 38.44710263-90, as well as other devices that provide the required test accuracy.

6.15. Measuring vessels of the required size can be selected from vessels that meet the requirements of the method according to GOST 20287 .

6.16. Gridand filter made of stainless steel or copper alloy made of wire with a diameter of 0.028 to 0.032 mm and a number of cells from 17,000 to 20,500 per 1 cmor N 0045 H according to GOST 6613 .

6.17. A cooling mixture consisting of solid carbon dioxide GOST 12162 or solid carbon dioxide obtained by throttling liquid carbon dioxide into a tight bag and rectified ethyl alcohol according to GOST 18300 or raw alcohol GOST 131 , or regenerated alcohol.

6.18. Thermometers type TINZ-1, TINZ-3, TN-8, GOST 400-80 .

6.19. Mechanical stopwatch.

7. SAMPLE PREPARATION

The test fuel sample is filtered through dry filter paper (section 5.3) at a temperature of at least 15 °C.

The fuel sample is taken GOST 2517 . To remove mechanical impurities and water, the fuel is filtered through a "white ribbon" filter at a temperature not less than 15 °C above the cloud point.

8. PREPARATION OF THE EQUIPMENT

Before each test, disassemble the filter (clause 6.7.2) and wash its parts, as well as the measuring vessel (clause 6.1), pipette (clause 6.7.1) and thermometer (clause 6.8) with solvent, then rinse with acetone and dry with clean dry air. Check the cleanliness and dryness of all parts and casing. Check that the filter mesh and connections are not damaged, if necessary, replace them with new ones. Then the equipment is assembled, as indicated in Fig.1. Check the tightness of the threaded nut (clause 6.7.2), if there is any leakage.

9. CONDUCTING THE TEST

9.1. The insulating ring (item 6.3) is placed on the bottom of the casing (item 6.2).

9.2. If the spacers (clause 6.4) are not made integral with the insulating ring (clause 6.3), they are placed at a distance of about 15 and 75 mm from the bottom of the measuring vessel (clause 6.1).

9.3. The measuring vessel is filled with the tested fuel up to the mark corresponding to 45 cm3.

9.4. The measuring vessel is closed with a cork with a pipette with a filter (p. 6.7) and an appropriate thermometer (p. 6.8) in it. If the limiting filterability temperature is expected to be below minus 30 °C, a thermometer with the lowest temperature limits is used. The thermometer must not be changed during the test.

The equipment is installed in such a way that the lower part of the filter (clause 6.7.2) is at the bottom of the measuring vessel; the thermometer is installed parallel to the pipette and in such a way that its lower end is (1.5 ± 0.2) mm from the bottom of the measuring vessel. The thermometer ball must not come into contact with either the wall of the measuring vessel or the filter.

9.5. The casing is placed vertically at a depth of (85 ± 2) mm in a cooling bath maintained at minus (34 ± 0.5) °C.

9.6. The measuring vessel is placed in the casing in a stable vertical position.

9.7. With the stopcock open (clause 6.10), the pipette is connected to the vacuum unit (clauses 6.11, 6.12) using flexible hoses attached to the tap (Fig. 1). Turn on the vacuum and adjust the airflow so that the U-gauge indicates a pressure drop of 200 mmH2O during the entire test.

9.8. The determination is started immediately after placing the measuring vessel in the casing. If the cloud point of the sample is known, it is allowed to start the determination at the moment when the sample is cooled to a temperature that is at least 5 °C higher than the cloud point. In the first stage of cooling, a bath with a temperature of minus (34 ± 0.5) ° C should always be used.

When the temperature of the sample reaches the appropriate value, install a stopcock (p.6.10) so that the filter is connected to a vacuum, causing the fuel sample to be sucked through the filter mesh into the pipette, at the same time start the stopwatch. When the fuel reaches the mark on the pipette, stop the stopwatch and set the valve in the initial position so that the sample can drain into the measuring vessel.

If the time to suck the fuel up to the mark exceeds 60 s, then the determination is stopped and repeated with a fresh mass for testing, starting from a higher temperature.

9.9. The operation (clause 9.8) is repeated after each decrease in the sample temperature by 1 °C until the temperature at which the flow through the filter stops or the pipette is not filled to the mark within 60 s is reached.

Record the temperature at the beginning of the last filtration.

9.10. If, after cooling in accordance with clauses 9.9 and 9.11 or 9.12, the sample fills the pipette up to the mark for no longer than 60 s, but does not flow back into the measuring vessel after the stopcock (clause 6.10) is set in its original position, then the temperature of the start of filtration must be recorded.

9.11. If at a temperature of minus 20 °C the flow of fuel through the filter does not stop, further cooling is carried out in a cooling bath with a temperature of minus (51 ± 1) °C or in an appropriately switched refrigerator and repeat the operation (clause 9.8) after each decrease in temperature by 1 ° FROM.

By changing the bath, the measuring vessel is quickly transferred to a new casing placed in the second cooling bath, or by adjusting the refrigerator.

9.12. If at a temperature of minus 35 °C the flow of fuel through the filter does not stop, further cooling is carried out in the third bath with a temperature of minus (67 ± 2) °C or by adjusting the refrigerator.

The kit is transferred as indicated in clause 9.11.

10. TEST REPORT

Record the temperature at the beginning of the last filtration to the nearest 1 °C (9.9 to 9.10) as the cold filterability limit temperature and refer to this standard.

Processing of results.

The result of the determination is taken as the arithmetic mean of the results of two consecutive determinations, rounded up to a whole number.

11. ACCURACY OF THE METHOD

The accuracy of the method is obtained by statistical examination of interlaboratory test results and is specified in paragraphs 11.1-11.2 (see note).

11.1. Convergence

The discrepancy between successive test results obtained by the same operator on the same apparatus under the same conditions on identical test material, when the test is correctly performed, exceeds the values ​​indicated in Fig. 9 in one case in twenty.

Damn.9. Error in determining the limiting filterability temperature on a cold filter

Error in determining the limiting filterability temperature on a cold filter

Note. Below minus 35 °С, the error is not established.

Two results of determinations obtained by one performer in one laboratory are recognized as reliable (with a confidence level of 95%) if the discrepancy between them does not exceed 1 °C.

11.2. Reproducibility

The discrepancy between two independent results obtained by different operators working in different laboratories on identical test material, if the test is correctly performed, exceeds the values ​​presented in Fig. 9 in one case in twenty.

Note. The accuracy data shown in Fig. 9 was obtained using a program using both automatic and manual methods.


Two test results obtained in two different laboratories are recognized as reliable (with a confidence level of 95%) if the difference between them does not exceed 2 °C.

APPENDIX. REQUIREMENTS FOR THERMOMETER FOR DETERMINATION OF THE LIMITING FILTERABILITY TEMPERATURE

APPENDIX

Crap.

The text of the document is verified by:
official publication
M.: Publishing house of standards, 1992

Official edition

COMMITTEE FOR STANDARDIZATION AND METROLOGY OF THE USSR Moscow

UDC v2MZ * - "2: Ov" LM Group * B19

STATE STANDARD OF THE UNION OF THE SSR

FUEL DIESEL

Method for determining the limiting temperature of the CCGT

filterability on a cold filter 1 "

diesel fuel*. Cold filter method 22254-92

for determination of low filtering temperature

OKSTU 02B1

Dot" shmlm

I. PURPOSE

This International Standard specifies a method for the determination of the cold filter plugging point of diesel and domestic heating oils intended for the national economy and for export.

Additions reflecting the needs of the national economy are in italics.

2. APPLICATION

The method applies to diesel fuels without additives and with additives, as well as fuels used in domestic heating systems.

3. DEFINITION

Filterability limit temperature (cold filter) - the highest temperature at which a given volume of fuel does not flow through a standardized filter unit for a certain time, during cooling under standardized conditions.

Official edition

© Standards Publishing, 1992

This standard cannot be completely million partially reproduced, replicated and distributed without the permission of the State Standard of the USSR

GOSG Ya22L4 ~ "S. f

4 ESSENCE OF THE METHOD

The method consists in the gradual cooling of the test fuel at intervals of I ® C and stoking it through a wire filter mesh at a vacuum of 1961 Pa (200 mm of water column)