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GB/T 260-2016 English PDF

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GB/T 260-2016: Test method for water in petroleum products -- Distillation method
Status: Valid

GB/T 260: Historical versions

Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB/T 260-2016359 Add to Cart 4 days Test method for water in petroleum products -- Distillation method Valid
GB/T 260-1977159 Add to Cart 2 days Determination of water content in petroleum products Obsolete

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GB/T 261   GB/T 259   GBZ/T 260   GB/T 262   

Basic data

Standard ID: GB/T 260-2016 (GB/T260-2016)
Description (Translated English): Test method for water in petroleum products -- Distillation method
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: E30
Classification of International Standard: 75.080
Word Count Estimation: 18,175
Date of Issue: 2016-12-13
Date of Implementation: 2017-07-01
Older Standard (superseded by this standard): GB/T 260-1977
Regulation (derived from): National Standard Announcement No.16 of 2016
Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China

GB/T 260-2016: Test method for water in petroleum products -- Distillation method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Test method for water in petroleum products--Distillation method ICS 75.080 E30 National Standards of People's Republic of China Replace GB/T 260-1977 Determination of water content of petroleum products Distillation (ISO 3733.1999, Petroleum products and bituminousmaterials- Determinationofwater-Distilationmethod, MOD) Released on December 13,.2016 2017-07-01 implementation General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China China National Standardization Administration issued

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 260-1977 "Measurement method for moisture content of petroleum products", major technical changes compared with GB/T 260-1977 as follows. --- Revised the standard name, modified from the "Measurement Method for Moisture Content of Petroleum Products" to "Determination of Distillation Method for Water Content of Petroleum Products"; --- In the scope of Chapter 1, the determination of tar and petroleum products and tar derivatives is added, and the determination of water content is specified. The circumference is not more than 25%, indicating the scope of investigation of precision; --- Add Chapter 2 normative references; --- The instrument has added specifications for the retort and receiver, and added an assembly schematic diagram of the retort receiver distillation unit 2 Table 1 of the receiver specifications; modified the length of the straight water condenser; add a note after 4.1, it is recommended that the interface of the glass instrument One adopts 19/24 Chapter 5 of the edition); ---In the result representation, increase the water content result by "volume fraction" or "mass fraction"; and increase the use of different specifications to receive , the accuracy requirements of the measurement results (see Chapter 10, Chapter 7 of the 1977 edition); --- Increased the precision of the method (see Chapter 11, Chapter 6 of the 1977 edition); --- Added normative Appendix A "Sample Processing". This standard uses the redrafting method to modify the use of ISO 3733.1999 "Petroleum products and asphalt materials in the determination of water content distillation law". This standard has a structural change compared with ISO 3733.1999. It will be reversed from Chapters 4 and 5, adding 4.3, 4.4, 4.6, 4.7, 8.5. 10.1 and 10.3. The main technical differences between this standard and ISO 3733.1999 and their reasons are as follows. --- Revised the standard name, modified from "Determination of Water Content in Petroleum Products and Bituminous Materials" to "Water Content of Petroleum Products" Determination of distillation method, because this standard does not include the content of water content determination of asphalt materials; --- This standard only uses the determination of water content in petroleum products and tars in ISO 3733.1999, involving asphalt materials. No content has been adopted, and the corresponding content of ISO 3733.1999 excluding emulsified products has not been adopted; --- Reference the corresponding national standards and industry standards in the normative reference documents; --- Considering the "marks" requirement of China's petroleum product indicators, GB/T 260- has been added to the specifications of the receivers in Table 1. The 10mL receiver specified in 1977, that is, the precision cone receiver, see Figure 3; --- Removed the detailed schematic diagram of the typical receiver of Figure 3 of ISO 3733.1999; --- Taking into account the "marks" requirements of China's petroleum product indicators, Chapter 5 "Reagents" revised the provisions on the solvent water content To modify the solvent as "solvent without water or water content not exceeding 0.02% by volume" as specified in ISO 3733.1999 Dehydrated and filtered before use, and determined by distillation, the water content determination result should be “None”; --- Add a note after 5.2, give the choice of commercial solvent or blended with the required petroleum fraction solvent; --- Added the calibration rule for the precision cone receiver between 0.0mL and 0.3mL in 6.2; --- Add a note after 8.4, indicating that when using a 10mL receiver to measure the sample, if the water content is greater than 10%, the sample can be reduced Quantity of treatment measures; --- Increase the test requirements when there are 8.5 trace indicators required; --- The representation of the calculation formula has been modified. Since the prescribed reagent blank is "none", the subtraction of the reagent blank is cancelled; --- In Chapter 10, the results of water content are indicated by "volume fraction" or "mass fraction"; the results of "marks" and "none" are added. Ming; and the use of precision cone receivers, the accuracy requirements of the measurement results; --- Added in 11.1 repeatability "When the water content is measured using a 10 mL precision cone receiver, the amount of water received by the receiver is When the concentration is 0.3mL or less, the difference between the obtained measurement results should not exceed one scale of the receiver"; --- Added references. This standard was proposed by the National Petroleum Products and Lubricants Standardization Technical Committee (SAC/TC280). This standard is governed by the National Petroleum Products and Lubricants Standardization Technical Committee Sub-Technical Committee on Petroleum Fuels and Lubricants (SAC/ TC280/SC1) is in charge. This standard was drafted by China Petroleum & Chemical Corporation Petrochemical Science Research Institute and Shenzhen Metrology Quality Inspection Institute. Yanshan Branch of China Petroleum & Chemical Corporation participated in the drafting. The main drafters of this standard. Gu Jie, Yan Yugui, Yang Tingting, Li Siyuan, Zhao Yan, Ling Liexiang, Ji Ming. The previous versions of the standards replaced by this standard are. ---GB/T 260-1964, GB/T 260-1977.

Introduction

Determination of the water content of petroleum products is very important for the refining, purchase, sale and transportation of petroleum products. The water content measured by this standard, It can be used for calibration when metering the petroleum products. Determination of water content of petroleum products Distillation WARNING. Use of this standard may involve certain hazardous materials, operations, and equipment, but does not address all safety issues associated with this. All made suggestions. Users are responsible for establishing appropriate safety and protection measures before applying this standard, and determining the appropriate regulatory restrictions. Use sex.

1 Scope

This standard specifies the method for determining the water content of petroleum products by distillation. This standard applies to petroleum products, tar and its derivatives. The water content is determined to be no more than 25%. This standard can measure samples with a water content of more than 25%, but its precision has not been examined. If a volatile water-soluble substance is present in the sample, it will be measured as water.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this article. Pieces. For undated references, the latest edition (including all amendments) applies to this document. GB 1922-2006 Solvent oil for paints and cleaning GB/T 4756 petroleum liquid manual sampling method (GB/T 4756-1998, eqvISO 3170. 1988) GB/T 6536 Determination of atmospheric distillation characteristics of petroleum products GB/T 15894-2008 Chemical reagent petroleum ether (ISO 6353-3.1987, NEQ) GB/T 27867 automatic sampling method for petroleum liquid pipelines (GB/T 27867-2011, ISO 3171.1988, IDT) SH/T 0229 Solid and semi-solid petroleum product sampling method

3 Method summary

The test sample and the water-incompatible solvent are heated and refluxed together, and the solvent can carry the water in the sample. Condensed continuously The solvent and water are separated in the receiver, water is deposited in a graduated receiver, and the solvent flows back to the distiller.

4 instruments

4.1 Overview The instrument includes a glass decanter, a graduated glass receiver, a reflux condenser, and a heater. Between the retort, receiver and condenser The connection should be sealed in a suitable manner, preferably with a ground connection. A typical assembly schematic is shown in Figures 1 and 2. Experimental instruments Matching, as described in 6.2 and 6.3, can give accurate results. Note. It is recommended that the interface of the glass instrument be unified 19/24 For the sample of the index, the scale is set to have a score of ten equal parts below 0.3 mL; a score of seven equal divisions is provided between 0.3 mL and 1.0 mL; 0.2 mL per division between 1.0 mL and 10 mL (see Figure 3). 4.4 condenser A straight water condenser with a length of 400 mm is recommended. 4.5 heater An electric heater can be used for the glass decanter, and an electric heater with magnetic stirring can be selected to prevent the boiling of the solution. 4.6 Balance The sensitivity is 0.1 g. 4.7 Measuring cylinder 4.7.1 10 mL graduated cylinder. The division value is 0.2 mL. 4.7.2 100mL graduated cylinder. The division value is 1mL. Table 1 Receiver specifications Receiver volume/mL 2 5 10 25 Scale range /mL 0~2 0~5 0~0.3 >0.3~1 >1~10 0~1 >1~10 0~10 0~1 >1~25 Minimum scale value/mL 0.05 0.05 0.03 0.1 0.2 0.1 0.2 0.1 0.1 0.2 Maximum scale error/mL 0.025 0.05 0.03 0.05 0.1 0.05 0.1 0.1 0.05 0.1 Receiver bottom shape rounded round precision cone (see Figure 3) Standard tapered circular cone Receiver scale section length Degree/mm 85~105120~140 85~105 120~140 120~140 140~160 Description. 1---distillation bottle; 2---receiver; 3---condenser. Figure 1 Distillation device without cock receiver Description. 1---condenser; 2---receiver; 3---distillation bottle; 4---cock. Figure 2 Distillation device with cock receiver The unit is mm Figure 3 10mL precision cone receiver

5 reagent

Use different extraction solvents depending on the sample (see 8.3). Refer to Table 3. The solvent should be dehydrated and filtered before use, according to 8.6~ The procedure of 8.9 determines the water content of the solvent and the result should be "none". 5.1 Aromatic solvent The aromatic solvents listed below can be used. a) xylene (mixed xylene) above industrial grade; b) a mixed solvent of 20% industrial grade toluene and 80% industrial grade xylene (mixed xylene); c) The petroleum fraction is tested in accordance with GB/T 6536, and its distillate at 125 ° C does not exceed 5% by volume, and the distillation at 160 ° C The yield is not less than 20% by volume, and the density at 20 ° C is not less than 852 kg/m 3 . 5.2 petroleum fraction solvent The petroleum fraction solvent is tested according to GB/T 6536, and the distillation temperature of 5% by volume is between 90 ° C and 100 ° C, and the volume is divided. The 90% distillation temperature is below 210 °C. Note. Petroleum ether in accordance with GB/T 15894-2008 at 90 °C ~ 120 °C, or petroleum ether at 90 °C ~ 120 °C and GB 1922- In.2006, the solvent oil No. 1 or No. 2 was formulated into a petroleum distillate solvent meeting the above requirements in an appropriate ratio. 5.3 paraffin-based solvent The water-free paraffin-based solvents listed below can be used. a) petroleum ether (light petroleum hydrocarbon) having a boiling point in the range of 100 ° C to 120 ° C; b) 2,2,4-trimethylpentane (isooctane) with a purity of 95% or more.

6 checksum recovery test

6.1 Overview Before the first use, verify the accuracy of the receiver according to 6.2. Use 6.3 for the recovery test before using the distillation unit. 6.2 Checking Before using for the first time, you need to verify the accuracy of the receiver scale, using a microtiter that can be read into 0.01mL, or use a 5mL micropipette, add distilled water to the receiver in increments of 0.03mL or 0.05mL each time, as appropriate The scale to be verified. If the difference between the added water value and the read water value exceeds 0.05 mL (for a 10 mL precision cone receiver Between 0.0mL and 0.3mL, if the difference between the added water value and the read water value exceeds 0.03mL), the receiver cannot be used. 6.3 Recovery test Before the moisture is measured using a distillation apparatus, it is necessary to perform a water recovery test on the entire distillation apparatus. According to the 500mL listed in 4.2~ A.2000 mL distillation flask is added with 250 mL to 1000 mL of xylene (5.1), and is operated according to Chapter 8. After the distillation is completed, discard Remove the solvent from the receiver. After the distillation bottle is cooled, add the appropriate amount of distilled water directly to the distillation bottle by pipette according to Table 2. Chapter 8 operates. If the volume of water obtained in the receiver meets the tolerances allowed in Table 2, it indicates that the test equipment meets the requirements. If the test results exceed the allowable error in Table 2, it is recommended to check whether there is steam leakage during the distillation process, the distillation speed is too fast, and the connection is too fast. The receiver is not accurately calibrated or has moisture ingress. After eliminating these influencing factors, re-verify and repeat the recovery test. Table 2 The allowable limit of water recovery is in milliliters The allowable limit of water recovery when the capacity of the receiver is 20 ° C at 20 ° C and the amount of water added to the distiller is 20 ° C 2 1.00 1.0±0.025 5 1.00 1.0±0.025 5 4.50 4.5±0.025 10 1.00 1±0.1 10 5.0 5±0.25 25 12.0 12±0.25

7 sampling

7.1 Overview Sampling is defined as obtaining a representative test specimen from a pipeline, tank or other system and placing it in a laboratory test vessel. All the steps required (see Appendix A). 7.2 Laboratory samples Unless otherwise specified, sampling shall be in accordance with GB/T 4756, GB/T 27867 or SH/T 0229. The amount of sample used for the test is determined based on the expected water content and the required water yield should not exceed the upper limit of the receiver scale. Unless received The unit has a cock that allows water out of the scale to be placed in a 10 mL graduated cylinder. 7.3 Preparation of test specimens In addition to the provisions of GB/T 4756, GB/T 27867 or SH/T 0229, the following steps are required to prepare samples. 7.3.1 Fragile solid samples shall be completely ground and mixed well. The sample used in the test should be obtained from it. 7.3.2 The liquid sample should be mixed in the original container and heated and mixed if necessary. Sample mixing time, mixing speed (speed) and agitation The height from the bottom of the sample container should be handled in accordance with Appendix A to allow the sample to meet analytical requirements. The volume and water content of the sample are not Should exceed the maximum value specified in Appendix A. Note. If there is any doubt about the uniformity of the sample mixed according to 7.3.1 or 7.3.2, if the sample amount is compatible with the expected water content when measuring the sample, All samples were measured at one time. If the sample size is large and cannot be measured at one time, at least 3 test samples are taken out, and 3 test results are recorded in the test. In the test report, the average of the results is taken as the result of the water content of the sample.

8 test steps

8.1 Before testing the sample, mix it according to step 7.3. 8.2 According to the type of sample, take an appropriate amount of the sample, accurate to ±1%, and transfer to the distillation flask according to 8.3 or 8.4 requirements. 8.3 For the flowing liquid sample, measure the appropriate amount of the sample in the measuring cylinder. Use a 50mL and two 25mL selected solvent (see section Chapter 5 and Table 3), flush the cylinders in portions and transfer all the samples to the distiller. After the sample is poured into the distiller or after each rinsing, the amount should be The tube is completely drained. Table 3 The sample to be tested is matched with the extraction solvent Extraction solvent type Aromatic solvent tar, tar products Petroleum fraction solvent fuel oil, lubricating oil, petroleum sulfonate, emulsified oil Paraffinic hydrocarbon solvent grease 8.4 For solid or viscous samples, weigh the sample directly into the retort and add 100 mL of the selected extraction solvent (see Table 3). For samples with low water content, it is necessary to increase the amount of sample, so the amount of solvent to be extracted also needs to be greater than 100 mL. Note. When using a 10mL receiver to test the sample, if the water content is greater than 10%, the amount of sample can be reduced so that the amount of distilled water does not exceed 10mL. 8.5 If the test sample has the requirement of “marks” of the product indicator, it is recommended to use a 10 mL precision cone receiver (see Figure 3). The amount of sample is 100 g or 100 mL, the amount of solvent added was 100 mL. 8.6 Magnetic stirring can effectively prevent bumping. Glass beads or boiling materials can also be added to the distiller to reduce bumping. 8.7 Assemble the distillation unit according to Figure 1 or Figure 2. By estimating the water content in the sample, select the appropriate receiver to ensure that the vapor and liquid are connected. The seal at the place. The condenser and receiver should be cleaned to ensure that the distilled water does not stick to the tube wall and all flows into the bottom of the receiver. in The top of the condenser is stuffed with loose cotton to prevent moisture from entering the atmosphere. Circulating cooling water is introduced into the jacket of the condenser. 8.8 Heat the distillation bottle and adjust the boiling rate of the sample so that the distillation rate of the condensate in the condenser is 2 drops/s~9 drops/s. Continue to distill to steam There is no more water in the distillation unit (except in the receiver) and the volume of water in the receiver remains unchanged within 5 min. If there is a water ring on the condenser, small The heart increases the distillation rate or turns off the circulation of the condensate for a few minutes. 8.9 After the receiver has cooled to room temperature, adhere the condenser tube to the receiver wall with a glass rod or Teflon rod, or other suitable tool. The water is transferred to the water layer. Read the water volume to the exact value. 8.10 If a new batch of solvent is used, the solvent required for the test shall be determined according to the procedure of 8.6~8.9. The water content determination result shall be “None”.

9 calculation

Calculate the volume fraction φ (%) or mass fraction of water in the sample according to the method of measuring the sample according to formula (1), formula (2) or formula (3). w (%). Φ= V1 V0× 100% (1) Φ= V1 m/ρ ×100% (2) w= V1ρ water m ×100% (3) In the formula. V0---the volume of the sample in milliliters (mL); V1---the moisture in the receiver when measuring the sample, the unit is milliliter (mL); m --- the mass of th......
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