GB/T 261-2008 Determination of flash point — Pensky-Martens closed cup method
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Card type: Test method
1. Method number / full title / English title / replacement relationship
- Standard number: GB/T 261-2008
- Chinese title: Determination of flash point — Pensky-Martens closed cup method
- English title: Determination of flash point—Pensky-Martens closed cup method
- Adoption relationship: modified adoption of ISO 2719:2002 (MOD)
- Replaces: GB/T 261—1983 "Petroleum products — Determination of flash point — Closed cup method"
- Previous versions: GB 261—1964, GB 261—1977, GB/T 261—1983
- Issued: 2008-08-25; implemented: 2009-02-01
- Proposed by / administered by: National Technical Committee for Standardization of Petroleum Products and Lubricants (administered by the Subcommittee on Petroleum Fuels and Lubricants)
- Drafting organization: Research Institute of Petroleum Processing, China Petroleum & Chemical Corporation
- Main drafters: Guo Tao, Chen Jie
2. Scope of application and exclusions
- Applicable to petroleum products, and also applicable to determination of flash point of chemical products such as varnishes and paints that do not form a surface film (from the foreword and Chapter 1).
- The test procedure is divided into Procedure A and Procedure B:
- Procedure A: applicable to paints and varnishes that do not form a surface film, unused lubricating oils, and other petroleum products not included in Procedure B.
- Procedure B: applicable to residual fuel oils, diluted bitumen, used lubricating oils, liquids that tend to form a surface film, liquids with suspended particles, and highly viscous materials (such as polymer solutions and adhesives).
- Note: When monitoring a lubricating oil system, to compare the flash points of unused and used lubricating oils, Procedure A may also be used to determine the flash point of used lubricating oil, but the precision of this standard applies only to Procedure B.
- Not applicable: liquids containing water or containing highly volatile materials.
- Note 1: The flash point of water-containing paints may be determined by GB/T 7634; the flash point of liquids containing highly volatile materials may be determined by ISO 1523 or GB/T 7634.
- Note 2: The precision data of this standard are valid only within the flash point range described in Chapter 13.
- Note 1 (scope): Although this standard may also be used for kerosene with a flash point above 40°C, in general the flash point of kerosene is determined according to ISO 13736; usually the flash point of unused lubricating oil is determined according to GB/T 3536.
- Note 2 (scope): This standard may also be used to determine jet fuels with a flash point below 40°C, but the precision has not been verified.
- Introduction note: The flash point test shall not be used for potentially unstable, readily decomposable, or explosive samples unless it has been confirmed in advance that they are safe at the temperatures specified in this standard; flash point test results obtained for samples containing halogenated hydrocarbons shall be analyzed with caution, because such samples may produce anomalous results.
3. Method principle
Pour the sample into the test cup, stir continuously at the specified rate, and heat the sample at a constant rate. At specified temperature intervals, with stirring interrupted, introduce an ignition source into the opening of the test cup so that the sample vapor flashes momentarily, and the lowest temperature at which the flash spreads over the liquid surface is the flash point at ambient atmospheric pressure; then use a formula to correct it to the flash point at standard atmospheric pressure. (Chapter 4)
4. Reagents and materials (purity / preparation)
- 5.1 Cleaning solvent: used to remove a small amount of sample adhering to the test cup and test cup lid.
- Note: The choice of cleaning solvent is based on the sample being tested and the stickiness of its residue. Low-volatility aromatic (benzene-free) solvents may be used to remove oil traces; mixed solvents such as toluene-acetone-methanol can effectively remove gum-like deposits.
- 5.2 Calibration liquid: see the provisions in Annex A.
- Specific purity and preparation concentration: not provided in the available source.
5. Apparatus and equipment
- 6.1 Pensky-Martens closed cup flash point tester: see Annex B.
- 6.1.1 When using an automatic instrument, ensure that its determination results can achieve the precision specified in this standard; the assembly of the test cup and test cup lid shall comply with the dimensions and mechanical requirements of the instrument specified in Annex B; the user shall ensure that all operations are carried out in accordance with the instrument instructions.
- Note: In some cases, test results obtained using electronic ignition and flame ignition may differ, and test results obtained using electronic ignition may be unclear in the source text (original text truncated here, requires confirmation against the source standard (source-text extraction)).
- 6.1.2 In cases of dispute, unless otherwise specified, the manual test result with flame ignition shall prevail for arbitration testing.
- 6.1.1 When using an automatic instrument, ensure that its determination results can achieve the precision specified in this standard; the assembly of the test cup and test cup lid shall comply with the dimensions and mechanical requirements of the instrument specified in Annex B; the user shall ensure that all operations are carried out in accordance with the instrument instructions.
- 6.2 Thermometers: including thermometers for low, medium, and high temperature ranges, meeting the requirements of Annex C. The thermometer shall be selected according to the expected flash point of the sample.
- Note: Other types of temperature measuring equipment may also be used, provided they can meet the accuracy and sensitivity of Annex C.
- 6.3 Barometer: accuracy 0.1kPa; barometers used by meteorological stations or airports that have been pre-calibrated to sea level readings shall not be used.
- 6.4 Heating bath or oven: used to heat the sample, required to control the temperature within ±5°C. It shall be ventilated and able to prevent flash ignition of combustible vapors generated when heating the sample; an explosion-proof oven is recommended.
- Annex B (normative) Key points of instrument structure:
- B.2 Test cup: made of brass or a non-corrosive metal with the same thermal conductivity, meeting the dimensional requirements of Figure B.2; the thermometer hole of the test cup shall be equipped with a device to position it in the heating chamber; preferably fitted with a handle but not so heavy as to tip an empty test cup.
- B.3.1 Test cup lid: made of brass or other non-corrosive metal with comparable thermal conductivity; there is a downward-hanging edge around the periphery, and the diametrical clearance between the hanging edge and the outer surface of the test cup shall not exceed 0.36 mm; the test cup lid has three openings A, B, C; the upper edge of the test cup shall be in close contact with the entire inner surface of the test cup lid.
- B.3.2 Sliding plate: made of brass about 2.4mm thick; operates on the upper surface of the test cup lid; when the sliding plate is turned to one end position, openings A, B, C are all closed, and when turned to the other end position, the three openings are all open; the mechanically operated sliding plate shall be spring type, with the three openings all closed when the sliding plate is not in use, and when operated to the other end position, the three openings are fully open and the tip of the igniter shall be able to descend fully into the test cup.
- B.3.3 Igniter: the tip opening diameter of the flame jet device of the ignition tube is about 0.7mm~0.8 mm; the tip is made of stainless steel or another suitable metal material; equipped with a mechanical operator, when the sliding plate is in the "open" position, lower the tip so that the center of the flame nozzle opening hole is located between the upper and lower surface planes of the test cup lid, and passes through a point on the radius of the center of the largest opening A.
- Note: The bead at the tip is made of a suitable material, comparable to the flame size (3mm~4mm), and may be mounted at a conspicuous position on the test cup lid.
- B.3.4 Automatic reignition device: used for automatic reignition of the flame.
- B.3.5 Stirring device: installed at the center of the test cup lid, with two double-blade metal paddles; the lower paddle surface is about 38 mm from the test cup lid, blade width 8 mm, inclined 45°; the upper paddle surface is about 19 mm from the test cup lid, blade width 8 mm, inclined 45°; the two sets of paddles are fixed on the rotating shaft of the stirrer; when viewed from below the stirrer, the two blades of one set of paddles are at positions 0° and 180°, and the other set is at positions 90° and 270°.
- Note: The rotating shaft of the stirrer may be connected to the motor by a flexible drive shaft or a suitable pulley assembly structure.
- B.4 Heating chamber and bath jacket: the heating chamber consists of an air bath and a bath jacket that can hold the test cup; the air bath has a cylindrical inner side and meets the requirements of Figure B.1; the air bath may be flame-heated type, electrically heated metal casting type, or resistance element heated type; the air bath shall ensure that it does not deform at the temperatures specified for the test.
- B.4.2.1 Flame-heated type or electrically heated metal casting type: the temperature of the bottom and side walls shall remain consistent, and the thickness of the air bath shall be not less than 6 mm; the design of the flame-heated casting shall ensure that flame combustion products cannot move up along the test cup wall or enter the test cup.
- B.4.2.2 Resistance element type: all parts of its surface are required to be heated uniformly, and the thickness of the walls and bottom of the air bath shall be not less than 6 mm.
- B.4.3 The bath jacket is made of metal, assembled so that there is a gap between the bath jacket and the air bath; the bath jacket may be mounted with three screws and gap bushings on unclear in the source text (original text truncated here, requires confirmation against the source standard (source-text extraction)).
- Annex C (normative) Thermometer specifications (Table C.1):
- Low range: temperature range −5~110°C; scale division 0.5°C; long line interval 1–5°C; numbered scale interval 5°C; indication tolerance 0.5°C; safety bulb permitted to be heated to 160°C; total length 282~295 mm; stem outer diameter 6.0–7.0 mm; temperature-sensing bulb length 9–13 mm; temperature-sensing bulb outer diameter 5.5~stem outer diameter; distance from bottom of temperature-sensing bulb to graduation line 0°C; scale range length 85–95 mm; stem expansion part outer diameter 7.5–8.5 mm, length 2.5~5.0 mm, distance from bottom to bottom of temperature-sensing bulb 64–66 mm.
- Medium range: temperature range 20–150°C; scale division 1°C; long line interval 5°C; numbered scale interval 5°C; indication tolerance 1.0°C; safety bulb permitted to be heated to 200°C; total length 282~295 mm; stem outer diameter 6.0–7.0 mm; temperature-sensing bulb length 9–13 mm; temperature-sensing bulb outer diameter 5.5~stem outer diameter; distance from bottom of temperature-sensing bulb to graduation line 20°C; scale range length 85–95 mm; stem expansion part outer diameter 7.5–8.5 mm, length 2.5–5.0 mm, distance from bottom to bottom of temperature-sensing bulb 64~66 mm.
- High range: temperature range 90–370°C; scale division 2°C; long graduation interval 10°C; numbered graduation interval 20°C; indication tolerance when <260: 1.0, when ≥260: 2.0; safety bulb allowed to be heated to 370°C; total length 282~295 mm; stem outer diameter 6.0–7.0 mm; temperature-sensing bulb length 7–10 mm; temperature-sensing bulb outer diameter 5.5~stem outer diameter; distance from bottom of temperature-sensing bulb to graduation line 90°C; scale range length 80–90 mm; stem expansion portion outer diameter 7.5–8.5 mm, length 2.5–5.0 mm, distance from bottom to bottom of temperature-sensing bulb 64~66 mm.
- Note 1: IP 15C/ASTM 9C; IP 16C/ASTM 10C; IP 101C and ASTM88C can meet the above requirements.
- Note 2: For the description of the low-range thermometer adapter, see Appendix D.
- Appendix D (informative) Thermometer adapter: Low-range thermometers sometimes need a metal sleeve to be fixed with the thermometer insertion hole used for the Tag flash point tester; the thermometer insertion hole of the Pensky-Martens closed-cup flash point tester is larger and requires an adapter to fit it; the dimensions of the thermometer adapter, sleeve, and gasket are shown in Figure D.1; the D.2 test gauge is used to measure the length of the stem expansion portion of the thermometer and the distance from the bottom of the temperature-sensing bulb to the bottom of the stem expansion portion (Figure D.2).
6. Recommended operating conditions
- Instrument placement: The instrument should be installed in a room without air flow and placed on a stable bench (7.1).
- Note 1: If air flow cannot be avoided, it is best to use a protective screen around the instrument.
- Note 2: If the sample produces toxic vapors, the instrument should be placed in a fume hood with independently controlled air flow, adjusted so that vapors can be drawn away, but the air flow must not affect the vapor above the test cup.
- Test cup cleaning: First rinse the test cup, test cup cover, and other accessories with cleaning solvent to remove all traces of gum or residue left from the previous test; then blow dry the test cup with clean air to ensure removal of the solvent used (7.2).
- Instrument assembly: Inspect the test cup, test cup cover, and accessories to ensure there is no damage and no sample deposit, then assemble the instrument according to Appendix B (7.3).
- Instrument calibration (7.4):
- 7.4.1 Calibrate the instrument at least once a year using certified reference materials (CRM) according to procedure A; the difference between the obtained result and the value given in CRM should be less than or equal to R/√2, where R is the reproducibility of this standard. It is recommended to use working reference samples (SWS) for frequent calibration of the instrument. For the recommended procedure for calibrating the instrument using CRM and SWS, and the method for obtaining SWS, see Appendix A.
- 7.4.2 The results obtained from calibration tests cannot be used as a bias of the method, nor can they be used for correction of subsequent flash point determination results.
- Procedure A operating conditions (10.2):
- Adjust the flame diameter to 3mm~4 mm; or turn on the electronic igniter and adjust the intensity according to the instrument manual.
- During the entire test, the sample is heated at a rate of 5 (°C/min)~6 (°C/min), and the stirring rate is 90 (r/min)~120 (r/min).
- Expected flash point not higher than 110°C: Start ignition from 23°C±5°C below the expected flash point, ignite once for every 1°C increase in sample temperature, and stop stirring during ignition.
- Expected flash point higher than 110°C: Start ignition from 23°C±5°C below the expected flash point, ignite once for every 2°C increase in sample temperature, and stop stirring during ignition.
- Ignition operation: Use the slide operation knob on the test cup cover or the ignition device to ignite, requiring the flame to descend into the vapor space of the test cup within 0.5s, and remain at this position for 1 s, then quickly rise back to the original position.
- Procedure B operating conditions (10.3):
- Adjust the flame diameter to 3mm~4mm; or turn on the electronic igniter and adjust the intensity according to the instrument manual.
- During the entire test, the sample is heated at a rate of 1.0 (°C/min)~1.5 (°C/min), and the stirring rate is 250 (r/min)±10 (r/min).
- Except that the stirring and heating rates are as specified in 10.3.2, all other test procedures are carried out as specified in 10.2.3~10.2.7.
7. Sampling and sample preparation
- 8.1 Unless otherwise specified, sampling should be carried out in accordance with GB/T 4756, SY/T 5317, or GB/T 3186.
- 8.2 (the text here is truncated in the source text, only “exceeding 30C” is seen, requires confirmation against the source standard (source-text extraction)).
- 9 Sample handling:
- 9.1 Petroleum products
- 9.1.1 Sample division: Carry out sample division at least 28°C below the expected flash point. If the divided samples are stored before testing, ensure that the sample fills more than 50% of the container volume.
- 9.1.2 Samples containing undissolved water: If the sample contains undissolved water, separate the water before mixing the sample, because the presence of water will affect the flash point determination result. However, free water in some residual fuel oils and lubricants may not be separable. In this case, physically remove the water before mixing the sample.
- 9.1.3 Samples that are liquid at room temperature: Before sampling, gently shake to mix the sample, then carefully sample, avoiding loss of volatile components as much as possible, then proceed according to Chapter 10.
- 9.1.4 Samples that are solid or semi-solid at room temperature: Place the container holding the sample into a heating bath or oven, heat at 30°C±5°C or at a temperature not exceeding the expected flash point 28°C (choose the higher temperature) 30 min, if the sample is not completely liquefied, heat again 30 min. However, avoid overheating the sample causing loss of volatile components, gently shake to mix the sample, then proceed according to Chapter 10.
- 9.2 Paints and varnishes: Sample preparation is carried out according to GB/T 20777.
- 9.1 Petroleum products
8. Analytical procedure
- 10.1 General: Residual fuel oil samples with high water content should be handled carefully, because after heating such samples will foam and overflow from the test cup.
- Note: The volume of the sample should be greater than 50% of the container volume, otherwise the flash point determination result will be affected.
- 10.2 Procedure A
- 10.2.1 Observe the barometer and record the ambient atmospheric pressure near the instrument during the test.
- Note: Although some barometers automatically correct, this standard does not require correction to atmospheric pressure under 0°C.
- 10.2.2 Pour the sample into the test cup to the filling line, cover the test cup cover, then place it into the heating chamber, ensure the test cup is in position or the locking device is connected, then insert the thermometer. Ignite the test flame source, and adjust the flame diameter to 3mm~4 mm; or turn on the electronic igniter and adjust the intensity of the electronic igniter according to the instrument manual. During the entire test, the sample is heated at a rate of 5 (°C/min)~6 (°C/min), and the stirring rate is 90 (r/min)~120 (r/min).
- 10.2.3 When the expected flash point of the sample is not higher than 110°C, start ignition from 23°C±5°C below the expected flash point, ignite once for every 1°C increase in sample temperature, and stop stirring during ignition. Use the slide operation knob on the test cup cover or the ignition device to ignite, requiring the flame to descend into the vapor space of the test cup within 0.5s, and remain at this position for 1 s, then quickly rise back to the original position.
- 10.2.4 When the expected flash point of the sample is higher than 110°C, start ignition from 23°C±5°C below the expected flash point, ignite once for every 2°C increase in sample temperature, and stop stirring during ignition. Use the slide operation knob on the test cup cover or the ignition device to ignite, requiring the flame to descend into the vapor space of the test cup within 0.5s, and remain at this position for 1 s, then quickly rise back to the original position.
- 10.2.5 When determining the flash point of an unknown sample, start the test at an appropriate initial temperature. Perform the first ignition at 5°C above the initial temperature, then proceed according to 10.2.3 or 10.2.4.
- 10.2.6 Record the temperature at which the ignition source causes obvious ignition inside the test cup as the observed flash point of the sample, but do not confuse the pale blue halo appearing around the test flame before the true flash point is reached with the true flash point.
- 10.2.7 If the difference between the recorded observed flash point temperature and the initial ignition temperature is less than 18°C or higher than 28°C, the result is considered invalid. Replace with a new sample and repeat the test, adjusting the initial ignition temperature until a valid determination result is obtained, that is, the difference between the observed flash point and the initial ignition temperature should be within the range of 18°C~28°C.
- 10.2.1 Observe the barometer and record the ambient atmospheric pressure near the instrument during the test.
- 10.3 Procedure B
- 10.3.1 (the text here is truncated in the source text, requires confirmation against the source standard (source-text extraction)).
- 10.3.2 Ensure the test cup is in position or the locking device is connected, then insert the thermometer. Ignite the test flame, and adjust the flame diameter to 3mm~4mm; or turn on the electronic igniter and adjust the intensity of the electronic igniter according to the instrument manual. During the entire test, the sample is heated at a rate of 1.0 (°C/min)~1.5 (°C/min), and the stirring rate is 250 (r/min)±10 (r/min).
- 10.3.3 Except that the stirring and heating rates of the sample are as specified in 10.3.2, all other test procedures are carried out as specified in 10.2.3~10.2.7.
9. Qualitative and quantitative determination and calculation formulas
- 11.1 Conversion of barometric pressure readings:
- Reading in hPa × 0.1= reading in kPa
- Reading in mbar × 0.1= reading in kPa
- Reading in mmHg × 0.1333= reading in kPa
- 11.2 Correction of observed flash point: Use formula (1) to correct the observed flash point to the flash point Tc under standard atmospheric pressure (101.3 kPa):
- Tc = To + 0.25(101.3 − p) …(1)
- Where: To—— observed flash point at ambient atmospheric pressure, °C; p—— ambient atmospheric pressure, kPa.
- Note: This formula is limited to atmospheric pressure within the range of 98.0kPa~104.7 kPa.
- 12 Expression of results: The result is reported as the flash point corrected to standard atmospheric pressure (101.3kPa), precise to 0.5°C.
10. Precision
Judge the reliability of test results (confidence level of 95%) according to the following provisions.
- 13.1 Repeatability, r: In the same laboratory, by the same operator using the same apparatus, following the same method, the difference between two consecutive test results on the same sample shall not exceed the values in Table 1 and Table 2.
- Table 1 Repeatability of procedure A:
- Paints and varnishes: flash point range not provided in the available source; r not provided in the available source.
- Distillate oils and unused lubricating oils: flash point range 40~250°C; r = 0.029X (X is the average of two consecutive test results).
- See also the value 1.5 in Table 1 (corresponding material/range requires confirmation against the source standard (source-text extraction)).
- Table 2 Repeatability of procedure B:
- Residual fuel oils and diluted bitumen: flash point range not provided in the available source; r = 2.0.
- Used lubricating oils: flash point range 40~110°C; r = 5 (a).
- Liquids tending to form a surface film, liquids with suspended particles, or highly viscous materials: flash point range 170~210°C; r = 5.0.
- a Results obtained in 20 laboratories on a used diesel engine oil sample.
- Table 1 Repeatability of procedure A:
- 13.2 Reproducibility, R:
- Note: The reproducibility of this precision does not apply to aviation lubricating oil No. 20.
- Table 3 Reproducibility of procedure A:
- Paints and varnishes: flash point range not provided in the available source; R not provided in the available source.
- Distillate oils and unused lubricating oils: flash point range 40~250°C; R = 0.071X (X is the average of two independent test results).
- Table 4 Reproducibility of procedure B:
- Residual fuel oils and diluted bitumen: flash point range not provided in the available source; R = 6.0.
- Used lubricating oils: flash point range 40~110°C; R = 16 (a).
- Liquids tending to form a surface film, liquids with suspended particles, or highly viscous materials: flash point range 170~210°C; R = 10.0.
- a Results obtained in 20 laboratories on a used diesel engine oil sample.
- Appendix A (informative) related to instrument verification:
- A.1.3 The evaluation of the accuracy of test results is based on a confidence level of 95%.
- A.2.1 Certified reference material (CRM): composed of stable pure hydrocarbons, in accordance with GB/T 15000.7 and GB/T 15000.3, or other stable petroleum products whose flash point by this standard has been determined through interlaboratory testing using the specified test method.
- A.2.2 Working reference sample (SWS): composed of stable petroleum products, pure hydrocarbons, or stable substances whose flash point has been determined by the following two methods.
- A.2.2.1 Using an instrument verified with CRM, conduct at least three tests on a representative sample, statistically analyze the results, remove outliers, and calculate the arithmetic mean of the results;
- A.2.2.2 Through a specific interlaboratory method involving at least three laboratories, repeated tests are conducted on representative samples, and the assigned flash point value can be obtained after calculating the interlaboratory statistical data.
- A.2.3 To ensure the integrity of SWS, SWS should be stored in a light-protected container, and the storage temperature of SWS should avoid exceeding 10°C.
- A.3.1 The flash point measurement range selected for CRM or SWS should meet the requirements of Table A.1; the reference values of flash point are given in Table A.1. To make the covered range as wide as possible, it is recommended to use two CRM or two SWS. The same CRM or SWS may also be used for repeated tests.
- A.3.2 For new instruments or in-use instruments used at least once a year, the instrument should be calibrated using CRM in accordance with the provisions of 10.2.
- A.3.3 For routine instrument verification, SWS may be used to perform calibration tests on the instrument in accordance with the provisions of 10.2.
- A.3.4 Correction for atmospheric pressure should be carried out in accordance with 11.2, and the corrected test result should be recorded, precise to 0.1°C.
- Table A.1 Reference values of closed-cup flash point for hydrocarbon samples:
- Decane: standard flash point 53°C
- Undecane: standard flash point 68°C
- Dodecane: standard flash point 84°C
- Tetradecane: standard flash point 109°C
- Hexadecane: standard flash point 134°C
- A.4.1.1 Single test: For a single test of CRM or SWS, the difference between the single result and the calibrated value of CRM or the assigned value of SWS shall satisfy the requirements of formula (A.1): |x − M| ≤ R/√2 … (A.1), where x— single test result; calibrated value of M—CRM or assigned value of SWS; R— reproducibility of this standard.
- A.4.1.2 (original formula number is A.2): |x̄ − M| ≤ R′/√n … (A.2), where x̄—average of test results; calibrated value of M—CRM or assigned value of SWS; R′—that is √[R² − r²(1 − 1/n)] (original source-text extraction is “VR 1 (1/n)”, requires confirmation against the source standard (source-text extraction)); R— reproducibility of this standard; r— repeatability of this standard; n— number of repeated tests using CRM or SWS.
- A.4.2 If the test results meet the above provisions, record them.
- A.4.3 For calibration verification using SWS, if the test results do not meet the above provisions, repeat the above steps using CRM. If the test results meet the above provisions, record them and delete the calibration result of SWS.
- A.4.4 If the test results still do not meet the above provisions, check whether the instrument and operation comply with the instrument manual. If there is no obvious inconsistency, use a different CRM for further calibration verification. If subsequent test results meet the above provisions, record them. If they still do not meet the above provisions, the instrument should be returned to the manufacturer for careful inspection.
11. Report
14 The test report shall include at least the following:
- State the standard implemented and the test procedure used;
- Type and complete identification of the product tested;
- If possible, report the preheating temperature and preheating time (see 9.1.4);
- Ambient atmospheric pressure near the instrument (see 10.2.1 and 10.3.1);
- Test results (see Chapter 12);
- Note any differences from the specified test procedure by agreement or for other reasons;
- Date of test.
12. Normative references
- GB/T 3186 Paints, varnishes and raw materials for paints and varnishes — Sampling (GB/T 3186—2006, ISO 15528:2000, IDT)
- GB/T 3536 Determination of flash and fire points of petroleum products — Cleveland open cup method (GB/T 3536—2008, ISO 2592:2000, MOD)
- GB/T 4756 Manual sampling of petroleum liquids (GB/T 4756—1998, eqv ISO 3170:1988)
- GB/T 6683 Determination of precision data for test methods of petroleum products (GB/T 6683—1997, neq ISO 4259:1992)
- GB/T 7634 Determination of low flash point of petroleum and related products — Rapid equilibrium method
- GB/T 15000.3 Directives for the work of reference materials (3) General principles and statistical methods for the certification of reference materials (GB/T 15000.3—1994, neg ISO Directive 35)
- GB/T 15000.7 Directives for the work of reference materials (7) General requirements for the competence of reference material producers (GB/T 15000.7—2001, ISO Directive 34, IDT)
- GB/T 15000.8 Directives for the work of reference materials (8) Uses of certified reference materials (GB/T 15000.8—2003, ISO Directive 33, IDT)
- GB/T 20777 Paints and varnishes — Examination and preparation of test samples (GB/T 20777—2006, ISO 1513:1992, IDT)
- SY/T 5317 Automatic pipeline sampling of petroleum liquids (SY/T 5317—2006, ISO 3171:1988, IDT)
- ISO 1523 Determination of flash point — Closed cup equilibrium method
- ISO 13736 Determination of flash point of petroleum products and other liquids — Abel closed cup method
- ASTM E1 ASTM Specification for liquid-in-glass thermometers
- IP Annual Book of Standards for Test Methods of Petroleum and Petroleum Products, Appendix A
13. Source and verification
This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.
14. Quick Q&A
| Question | Key answer points |
|---|---|
| Which version does this standard replace? | Replaces GB/T 261—1983; previous versions GB 261—1964, GB 261—1977, GB/T 261—1983. |
| Adoption of international standard? | Modified adoption of ISO 2719:2002 (MOD). |
| Dates of publication and implementation? | Published on 2008-08-25, implemented on 2009-02-01. |
| Which samples is it applicable to? | Petroleum products, and chemical products such as varnishes and paints that do not form a surface film. |
| Which samples is it not applicable to? | Water-containing paints or liquids containing highly volatile materials. |
| What does step A apply to? | Paints and varnishes that do not form a surface film, unused lubricating oils, and other petroleum products not included in step B. |
| What does step B apply to? | Residual fuel oils, diluted bitumen, used lubricating oils, liquids that tend to form a surface film, liquids with suspended particles, and highly viscous materials. |
| What is the basis for the arbitration test? | The result of the manual test ignited with a flame ignition source (6.1.2). |
| Heating rate and stirring rate for step A? | 5–6 °C/min; 90–120 r/min. |
| Heating rate and stirring rate for step B? | 1.0~1.5 °C/min; 250 r/min±10 r/min. |
| Diameter of the ignition flame? | 3mm~4 mm. |
| Flame descent and dwell time during ignition? | Lower into the vapor space within 0.5s, dwell for 1 s, then quickly raise back to the original position. |
| Ignition interval when the expected flash point is ≤110°C? | Ignite once for every increase of 1°C, starting from 23°C±5°C below the expected flash point. |
| Ignition interval when the expected flash point is >110°C? | Ignite once for every increase of 2°C, starting from 23°C±5°C below the expected flash point. |
| Requirement for a valid result regarding the difference between the observed flash point and the initial ignition temperature? | It should be within the range of 18°C~28°C; otherwise the result is invalid. |
| Barometric pressure correction formula? | Tc = To + 0.25 (101.3 − p), limited to 98.0~104.7 kPa. |
| To what precision is the result reported? | Corrected to 101.3 kPa, accurate to 0.5°C. |
| Instrument calibration frequency and criteria? | Use CRM according to step A to calibrate at least once a year; the difference between the result and the value given by CRM is ≤R/√2. |
| For which sample type is the precision not applicable? | The reproducibility is not applicable to 20 aviation lubricating oil. |
| What should the test report at least include? | Standard and procedure, product type identification, preheating temperature/time (if possible), ambient atmospheric pressure, test results, explanation of differences, test date. |
| Which standards are referenced for sampling? | GB/T 4756, SY/T 5317, or GB/T 3186. |
| Reference for the preparation of paint and varnish samples? | GB/T 20777. |
| How many temperature ranges does the thermometer have? | Three temperature ranges: low, medium, and high, selected according to the expected flash point. |
| Barometer accuracy requirement? | 0.1kPa, a barometer that has been pre-calibrated to sea level readings must not be used. |
| Temperature control requirements for the heating bath/oven? | Controlled within ±5°C, an explosion-proof oven is recommended. |
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