GB/T 18612-2011 English PDFUS$299.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 18612-2011: Determination of organic chloride content in crude oil Status: Valid GB/T 18612: Historical versions
Basic dataStandard ID: GB/T 18612-2011 (GB/T18612-2011)Description (Translated English): Determination of organic chloride content in crude oil Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: E21 Classification of International Standard: 75.040 Word Count Estimation: 13,193 Date of Issue: 2011-09-29 Date of Implementation: 2012-01-01 Older Standard (superseded by this standard): GB/T 18612-2001 Quoted Standard: GB/T 4756, GB/T 6536, GB/T 6682, SY/T 5317 Adopted Standard: ASTM D4929-2007, MOD Regulation (derived from): National Standards Bulletin 2011 No. 14 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 Summary: This standard specifies the determination of crude organic chlorine content in two ways. Including the method A biphenyl sodium reduction potentiometric titration and Method B microcoulometry combustion oxidation method. This standard applies to the determination of organic chlorine content greater than 1��g/g of crude oil. Method B does not apply where the total sulfur -containing organic chlorine content greater than Kin 10, 000 times the crude oil. GB/T 18612-2011: Determination of organic chloride content in crude oil---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.Determination of organic chloride content in crude oil ICS 75.040 E21 National Standards of People's Republic of China Replacing GB/T 18612-2001 Determination of organic chloride content of crude oil Issued on. 2011-09-29 2012-01-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released ForewordThis standard was drafted in accordance with GB/T 1.1-2009 given rules. This standard replaces GB/T 18612-2001 "crude organic chloride content measured microcoulometry Law", and GB/T 18612-2001 Compared to the main technical changes are as follows. --- Standard name from "crude organic chloride content measured microcoulometry Act" to "Determination of organic chloride content of crude oil"; --- Increased Chapter 5, "Method A --- sodium biphenyl reduction potentiometric titration"; --- Revised Chapter 6, "Method B --- combustion oxidation microcoulometry Law" precision (2001 Version 15.1; edition 6.5.1); --- Increased Chapter 7, "quality assurance and control." This standard uses redrafted law revision adopted ASTMD4929-07 "Determination of organic chloride content of crude oil." This standard ASTMD4929-07 compared to the structure have more adjustment, listed in Appendix A of this standard and ASTMD4929-07 The reg number control list. This standard also made the following editorial changes. --- Delete Chapter 4 ASTMD4929-07 the "meaning and purpose"; --- Chapter 25 ASTMD4929-07 delete "key words"; --- Added "Test Report" (Chapter 8 of this standard); --- Remove the informative annex ASTMD4929-07. The standard proposed by China National Petroleum Corporation. This standard by the National Standardization Technical Committee of Oil and Gas (SAC/TC355) centralized. This standard was drafted. Daqing Oilfield Engineering Co., Ltd. China Petrochemical Research Institute of Petroleum, China PetroChina Pipeline Company Pipeline Technology Research Center. The main drafters of this standard. Wei Che-ho, Zhanghan Pei, Pei Ho, Zhang, Wang Yuanfeng, Wen Yong. Determination of organic chloride content of crude oil Warning --- personnel should use this standard regular laboratory work experience. This standard does not point out all possible security asked question. Users have the responsibility to take appropriate safety and health practices and to ensure compliance with the conditions relevant national regulations.1 Scope1.1 standard specifies the determination of organic chloride content of crude oil in two ways. Method A --- including biphenyl and sodium reduction potentiometric titration Method B --- microcoulometry combustion oxidation method. 1.2 This standard applies to the determination of organic chlorine content is more than 1μg/g of crude oil. Method B does not apply where the total sulfur content of more than chlorine-containing organic 10,000 times the amount of crude oil.2 Normative referencesThe following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document. GB/T 4756 petroleum liquids hand sampling method (GB/T 4756-1998, ISO 3170. 1988, eqv) GB/T 6536 Petroleum products - Determination of distillation (GB/T 6536-1997, ASTMD86.1995, eqv) GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD) SY/T 5317 petroleum liquids pipeline automatic sampling (SY/T 5317-2006, ISO 3171. 1988, IDT) Principle 3 3.1 naphtha fraction obtained by crude distillation 204 ℃ before the distillation process should be GB/T 6536 requirements execution. With naphtha fraction Base and sufficient water elution to remove hydrogen sulfide and inorganic chlorides contained. 3.2 Determination of the following two methods naphtha fraction eluted after organochlorine content. 3.2.1 Method A. Transfer by naphtha fraction after elution to a separatory funnel containing dissolved sodium in toluene biphenyl. There may be sodium biphenyl Organic halide is converted to inorganic halides, the aqueous phase is concentrated by evaporation, addition of acetone potentiometric titration, to calculate the crude organic chloride content. Crude organic bromide and iodide of the organic method influential. 3.2.2 Method B. injected to contain about 80% oxygen and 20% of an inert gas (for example, by a naphtha fraction after elution. helium, argon Air or nitrogen) the gas flow through the tube 800 ℃ pyrolysis temperature of the organic chlorine into chlorides and oxychlorides, and silver ions in the titration cell Sub reaction. Consumed by the electrolysis silver ion Coulomb meter supplement, the total power consumption of silver ions added is calculated based on the crude oil Organochlorine content. Crude organic bromide and iodide of the organic method influential. Chloride titration cell reaction is as follows. Cl- Ag → AgCl ↓ Coulomb reaction of the silver ions consumed in the reaction occurs as follows. A → g Ag e-4 crude and distillate purification4.1 Reagents and materials Unless otherwise specified in the analysis using only analytical reagent. 4.1.1 potassium hydroxide (KOH). Warning --- may cause severe skin burns. 4.1.2 acetone (CH3COCH3). Warning --- flammable and may cause fire, harmful to health. 4.1.3 toluene (C6H5CH3). Warning --- flammable, harmful to health. 4.1.4 Water. in line with GB/T 6682 in two water requirements. 4.1.5 potassium hydroxide solution. c (KOH) = 1mol/L. 4.1.6 filter paper. 4.2 Instrument 4.2.1 round-bottomed distillation flask. heat-resistant glass, volume 1L, short bottleneck and has a 24/40 ground glass outside interface. 4.2.2 T-type takeover. heat-resistant glass, with a branch pipe 75 °, with 24/40 ground glass interface. 4.2.3 Thermometer. temperature range of 0 ℃ ~ 300 ℃, the minimum scale of 1 ℃. 4.2.4 Thermometer Interface. heat-resistant glass, with 24/40 ground glass inside interface. 4.2.5 Straight condenser. heat-resistant glass, 300mm, with a 24/40 ground glass interface. 4.2.6 evacuated Interface. heat-resistant glass, bent 105 °, with a 24/40 ground glass interface. 4.2.7 receiving cylinder. heat-resistant glass, the volume of 250mL, with a 24/40 ground glass outside interface. 4.2.8 Metal clip. for the 24th ground glass interfaces, stainless steel. 4.2.9 The cooling bath. the volume of 4L. 4.2.10 brass. for heat exchange cooling condensate, an outer diameter of 6.4mm, the length of 3m. 4.2.11 electric heating mantle. volume 1L, 0W ~ 1000W adjustable. 4.2.12 electronic balance. accurate to 0.01g. 4.3 Sampling This standard should be GB/T 4756 or SY/T 5317 to obtain a representative sample. 4.4 Preparation of the sample 4.4.1 All glassware should be washed successively with toluene and acetone, and then dried with a stream of dry nitrogen. Weigh and record the round-bottomed flask and then The reception quality of the cylinder. Install glass distillation apparatus, sealed with Vaseline all interfaces, then the metal clip it interfaces, interfaces to prevent loosening. in When you install a thermometer, see GB/T 6536 Fig. 1, adjusted T-takeover position within the thermometer, so that the bottom end of the connection capillary thermometer cold T-takeover highest level of the bottom wall of the condenser. 4.4.2 The copper tube is wound into a coil, mounted inside the cooling bath, cooling bath in the center of the cylinder to make room for the reception. PTFE tube Brass reels one end connected to a water source, the lower branch pipe connected to the other end of the straight tube condenser of the condenser bushing on the branch pipe connected to the drain Place. The mixture was cooled with ice-water bath was filled, circulating open water, the condenser temperature should be kept below 10 ℃. 4.4.3 The crude oil was added about 500mL weighed round bottom flask, weigh and record crude oil quality, accurate to 0.1g. The flask with steam Distillate device is connected, is placed in an electric heating mantle, the reception has been weighing on the cylinder below the outlet distillate, turn power electric heating mantle, distillation. Distillation process, by regulating the electric heating mantle knob to control distillation rate of about 5mL/min. When the thermometer reading reaches 204 ℃, Receiving cylinder removed, distillation was stopped. Weigh and record the distillate quality material, accurate to 0.1g. 4.4.4 The naphtha fraction is transferred from the receiving cylinder to a separatory funnel, potassium hydroxide solution with an equal volume (4.1.5) washed three times with oscillation, Removing hydrogen sulfide, then with an equal volume of water (4.1.4) oscillation washed three times to remove traces of inorganic chloride. Naphtha distillates washed Sub-filter to remove excess water and store in a clean glass jar and set aside. 4.5 Calculation Results 4.5.1 naphtha fraction mass fraction f, expressed in%, according to equation (1). f = mnmc (1) Where. Numerical mn --- collected naphtha fraction of the mass in grams (g); Quality mc --- crude oil values in grams (g). 4.5.2 extracted with a known amount of mass 10mL 10mL volumetric flask naphtha fraction, weighed to the nearest 0.1g. The density of the naphtha fraction D, Values in grams per milliliter (g/mL) said, according to the formula (2). D = mV (2) Where. Numerical m --- naphtha fraction of the mass in grams (g); Numerical V --- naphtha fraction of the volume, in milliliters (mL). 5 Method A --- sodium biphenyl reduction potentiometric titration 5.1 Reagents and materials Unless otherwise specified in the analysis using only analytical reagent. 5.1.1 Silver nitrate (AgNO3). 5.1.2 nitric acid (HNO3). Warning --- corrosive and may cause severe skin burns. 5.1.3 isopropanol ((CH3) 2CHOH). Warning --- flammable, harmful to health. 5.1.4 iso-octane (C8H18). 2,2,4- trimethyl pentane. Warning --- flammable, harmful to health. 5.1.5 biphenyl sodium (C12H10Na). using 15mL plastic bottle, a plastic bottle using the full dose of each test, each Plastic bottles are active 13mg ~ 15mg of sodium. Sodium biphenyl reagent should be stored at low temperatures, but not frozen. Prior to use, Reagent heated to about 50 ℃, sufficiently shaken to ensure homogeneity. 5.1.6 standard silver nitrate solution. c (AgNO3) = 0.01mol/L. 5.1.7 nitric acid solution. c (HNO3) = 5mol/L. The 160mL nitrate (5.1.2) was added to 200mL water (4.1.4), and then diluted To 500mL. 5.1.8 Congo red. 5.2 Instrument 5.2.1 General glass electrode. When repeatedly using an electrode, the electrode should be weekly washed once with chromic acid lotion, or by other strong oxidizing Agent lotion. Warning --- chromic acid lotion is a strong oxidant, can cause severe burns, cancer. 5.2.2 silver - silver chloride electrode. 5.2.3 potentiometric titrator. with a capacity not greater than 5mL burette and magnetic stirrer. 5.2.4 Electronic balance. accurate to 0.01mg. 5.3 Analysis Steps 5.3.1 Prior to the determination of chloride, all glassware should be washed with water, then rinsed with acetone. 5.3.2 50mL toluene injection volume of 250mL separating funnel, and adding a plastic bottle biphenyl sodium (5.1.5), mixed well Together, then add the sample obtained by the 4.4.4 about 30g, accurate to 0.1g. The funnel was Gaiyan and mixed solution or suspension should form Now blue-green, or should be added sodium biphenyl a plastic bottle until a solution or suspension of blue-green. 5.3.3 After the solution was mixed well, then placed 10min, waiting for the end of the completion of the reaction, and then successively added 2mL isopropanol, gently open Shaken until the solution color from blue to green to colorless. Then added 20mL of water and 10mL of nitric acid solution (5.1.7) and gently shake Do not swing through the cock relief. Congo red test paper with the aqueous phase, if there is no paper turns blue, then added a solution of nitric acid 5mL, straight Blue paper to date. 5.3.4 The aqueous phase was transferred to another isooctane containing 50mL separatory funnel, shake well after the aqueous phase was transferred to a 250mL burning Cup. Has been used a few drops of nitric acid solution 25mL water sample containing isooctane secondary extraction, the aqueous phase is also transferred to 250mL beaker, the beaker was heated on a hot plate in an aqueous solution was evaporated to 25mL ~ 30mL. Heating plate temperature should be maintained at Below the boiling point of the solution, the solution to avoid boiling. 5.3.5 After cooling the solution was added 100mL of acetone, potentiometric titration with silver nitrate standard solution (5.1.6). If you use automatic electrical Bit titrator is used Semimicro 5mL burette; if you are using a manually operated titrator, the semi-micro 5mL burette should be accurate Second place after the decimal point. 5.3.6 With manual titration, the titration end point may be determined by the method of drawing the titration curve, the titration curve represents the measured potential and consumption Silver nitrate solution corresponding relationship between the volume; When using automatic titration, the titration end point is the inflection point of the titration curve. 5.3.7 should be blank, blank solution should include all reagents except the sample. 5.4 Calculation Results 5.4.1 naphtha fraction of organic chlorine content of the mass fraction wn and its value in micrograms per gram (μg/g) expressed by the formula (3) Calculated. wn = (V1-V2) c × 35460 m1 (3) Where. Value Vl --- titration volume when consumed sample standard silver nitrate solution, in milliliters (mL of); The value of the volume V2 of the blank test --- consumed standard silver nitrate solution, in milliliters (mL of); Numerical c --- silver nitrate standard solution molar concentration, measured in moles per liter (mol/L); Numerical mass m1 --- sample in grams (g); 35460 --- conversion factor. 5.4.2 Crude organic chloride content in mass fraction w and its value in micrograms per gram (μg/g) expressed by the formula (4) Calculated. w = wn × f (4) Where. wn --- naphtha fraction of the value of organic chloride content (5.4.1), in micrograms per gram (μg/g); f --- naphtha fraction mass fraction (4.5.1). 5.5 precision and departing 5.5.1 Precision 5.5.1.1 Repeatability (r) In the same laboratory by the same operator using the same equipment, according to the provisions of the standard operation, and in a short time of each other the same sample Independent tests conducted two independent test results obtained absolute difference does not exceed the probability according to equation (5) to calculate the value of 95%. r = 0.32 (X 0.33) 0.644 (5) Where. The arithmetic average of crude oil of organic chloride content X --- twice as measured in micrograms per gram (μg/g). 5.5.1.2 Reproducibility (R) In different laboratories by different operators using different equipment, according to the provisions of the standard operation, independent of each other into the same sample The absolute difference between two independent test results obtained in the test line does not exceed the probability according to equation (6) to calculate the value of 95%. R = 0.7 (X 0.33) 0.644 (6) Where. The arithmetic average of crude oil of organic chloride content X --- twice as measured in micrograms per gram (μg/g). 5.5.2 deviate Crude oil was added to a variety of known content of various organic chlorine compounds, conduct recovery test. The amount of deviation shown in Fig. An organic chlorine content of a recovery curve 6 Method B --- combustion oxidation method microcoulometry 6.1 Reagents and materials Unless otherwise specified in the analysis using only analytical reagent. 6.1.1 Reaction gas. oxygen, high-purity grade. 6.1.2 Carrier gas. argon, helium, nitrogen or carbon dioxide, high purity grade. 6.1.3 silver acetate (CH3COOAg). 6.1.4 glacial acetic acid (CH3COOH). 6.1.5 chlorobenzene (C6H5Cl). 6.1.6 acetic acid solution. volume fraction of 70%. The 300mL water (4.1.4) and 700mL glacial acetic acid (6.1.4) and mix well. 6.1.7 chlorine standard stock solution. a chlorine content of 1000mg/L. Accurately weigh 1.587g chlorobenzene (6.1.5) in 500mL volumetric flask Isooctane (5.1.4) diluted to the mark. 6.1.8 chlorine standard solution. chlorine content of 10mg/L. Pipette 1.0mL chlorine standard stock solution (6.1.7) in 100mL volumetric flask Isooctane diluted to the mark. 6.2 Instrument 6.2.1 cracker. thermostat can be 800 ℃. 6.2.2 quartz pyrolysis tube. the inlet section should be used for the injection syringe septum, and the reaction gas can be introduced into the intake manifold and a carrier gas. Sample inlet section can be completely evaporated, the carrier gas evaporated sample loading oxidation zone, in the oxidation zone with the reaction gas mixture and combustion, combustion tube The oxidation zone should have sufficient space to ensure complete combustion of the sample. 6.2.3 Titration pool. comprises detecting changes in the concentration of silver ion sensing - reference to the electrode; to maintain a constant concentration of silver ion generator Yang - cathode On; vias imported gas obtained from the pyrolysis tube samples. Sensing electrode, a reference electrode and an anode made of silver electrode generator, generator overcast Pole made of platinum wire. Reference electrode immersed in a saturated solution of silver acetate, acetic acid electrolyte solution (6.1.6). 6.2.4 microcoulometry. a continuously adjustable gain and bias control, the sensor is able to measure - the difference between the reference potential electrode pair ratio and the potential difference And the bias potential is compared, then the comparison value is applied to the larger generator male - cathode pair titration. The output signal microcoulometry Proportional to the current generated. Microcoulometry may have a digital instrument and electrical systems, the output signal is directly converted into organic chlorine The number of nanograms or micrograms. 6.2.5 Sample syringe. volume of 50μL micro syringe. Can accurately sample 5μL ~ 50μL injected into the pyrolysis tube. Recommended 75mm ~ 150mm long needle, the sample is injected into the cracking tubes in the inlet section of about 500 deg.] C. 6.2.6 Injector. Recommended injection speed does not exceed 0.5μL/s. 6.3 Analysis Steps 6.3.1 The device according to the manufacturer's instructions to install the equipment. 6.3.2 Typical operating conditions are as follows. The reaction gas (O2) flow rate. 160mL/min Carrier gas flow rate. 40mL/min Oven temperature. Entrance. 700 ℃ Middle and outlet. 800 ℃ Microcoulometry. Bias. 240mV ~ 265mV Gain. about 1200 6.3.3 sample syringe 30μL secondary distilled or deionized water injected directly into the titration cell, increase or decrease the bias, making due The total integrated value of the minimum dilution effect arising. 6.3.4 extracted with 50μL 30μL ~ 40μL syringe samples obtained from the 4.4.4, carefully remove air bubbles, withdraw the needle bar so that the meniscus 5μL reached the lowest point at the other end of the liquid column syringe record readings. After injection of the sample, pull out the syringe, then withdraw the needle bar so that the recess Level the lowes......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 18612-2011_English be delivered?Answer: Upon your order, we will start to translate GB/T 18612-2011_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. 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