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GB/T 6324.10-2020: Test method of organic chemical products - Part 10: Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method
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Test method of organic chemical products - Part 10: Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method
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GB/T 6324.10-2020
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Basic data | Standard ID | GB/T 6324.10-2020 (GB/T6324.10-2020) | | Description (Translated English) | Test method of organic chemical products - Part 10: Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G15 | | Classification of International Standard | 71.080.01 | | Word Count Estimation | 7,726 | | Date of Issue | 2020-03-31 | | Date of Implementation | 2021-02-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 6324.10-2020: Test method of organic chemical products - Part 10: Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method
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Test method of organic chemical products - Part 10.Determination of trace sulfur in organic liquid products - Ultraviolet fluorescence method
ICS 71.080.01
G15
National Standards of People's Republic of China
Test methods for organic chemical products
Part 10.Organic Liquid Chemical Products
Determination of trace sulfur by ultraviolet fluorescence method
2020-03-31 released
2021-02-01 implementation
State Administration for Market Regulation
Issued by the National Standardization Management Committee
Foreword
GB/T 6324 "Test Methods for Organic Chemical Products" is divided into the following parts.
---Part 1.Water miscibility test of liquid organic chemical products;
---Part 2.Determination of the dry residue after evaporation of the volatile organic liquid on the water bath;
---Part 3.Determination of reduced potassium permanganate substances;
---Part 4.Determination of trace sulfur in organic liquid chemical products by microcoulometric method;
---Part 5.Determination of carbonyl compound content in organic chemical products;
---Part 6.Determination of the color of liquids, tristimulus value colorimetry;
---Part 7.Determination of melting color;
---Part 8.Determination of Moisture in Liquid Products by Karl Fischer Coulometric Method;
---Part 9.Determination of chlorine;
---Part 10.Determination of trace sulfur in organic liquid chemical products by ultraviolet fluorescence method.
This part is Part 10 of GB/T 6324.
This section was drafted in accordance with the rules given in GB/T 1.1-2009.
This part was proposed by the China Petroleum and Chemical Industry Federation.
This part is under the jurisdiction of the National Chemical Standardization Technical Committee (SAC/TC63).
Drafting organizations of this section. China Petroleum & Chemical Corporation Beijing Research Institute of Chemical Industry, Luxi Group Co., Ltd., PetroChina
Gas Co., Ltd. Jinzhou Petrochemical Company, China National Petroleum Corporation Jilin Petrochemical Company, China Petrochemical Corporation
Co., Ltd. Shanghai Petrochemical Research Institute, Quzhou Fluorosilicon Technology Research Institute.
The main drafters of this section. Li Sirui, Pang Yuna, Huang Yu, Zhao Jian, Ren Xufan, Xu Jingzao, Jiang Jianzhun, Zhong Jun, Sun Caihong, Wang Chuan, Li Xianzhong,
Gong Bin, Tian Liang.
Test methods for organic chemical products
Part 10.Organic Liquid Chemical Products
Determination of trace sulfur by ultraviolet fluorescence method
Warning---Excessive exposure to ultraviolet light is harmful to health, and the tester should avoid direct exposure to ultraviolet light and secondary or scattered radiation.
All parts of the body, especially the hazards of the eyes.
1 Scope
This part of GB/T 6324 specifies a method for the determination of total sulfur in organic liquid chemical products using ultraviolet fluorescence.
This section applies to the determination of organic liquid chemical products with sulfur content ranging from 0.2mg/kg to 100mg/kg.
This section does not apply to the determination of sulfur in organic liquid chemical products containing nitrogen, halogen, phosphorus, and silicon.
Note. If the sulfur content in the product is low, and the nitrogen or halogen content is high, the nitrogen or halogen content will affect the sulfur determination results.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 3723 General Rules for Sampling Safety of Industrial Chemical Products
GB/T 6680 General Rules for Sampling of Liquid Chemical Products
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Principles of the method
The liquid sample is injected into the combustion tube, mixed with oxygen and burned, and the sulfide in the sample is mainly converted into sulfur dioxide, which is brought into the test by the carrier gas
After being irradiated by an ultraviolet lamp, sulfur dioxide absorbs ultraviolet light energy and converts it into excited sulfur dioxide (SO2*). Excited Sulfur Dioxide Return
The fluorescence emitted when returning to the stable state of sulfur dioxide is amplified by the photomultiplier tube, detected by the photon counter, and the sulfur standard curve is used.
The obtained signal value calculates the sulfur content of the sample.
4 Reagents and materials
4.1 Carrier gas. argon or helium, with a purity of not less than 99.99% (volume fraction).
4.2 Oxygen. The purity is not less than 99.99% (volume fraction).
4.3 Thiophene (C4H4S) or dibenzothiophene (C6H4C6H4S). analytically pure, with a purity of not less than 98% (mass fraction), used to prepare sulfur standards
Quasi solution.
4.4 Solvent. analytical grade. Isooctane, toluene, etc., or other solvents similar to the sample to be tested, are used to prepare standard solutions and dilute samples.
The sulfur content in the solvent should not be higher than 0.2mg/kg, and the sulfur content of the selected solvent should be blank corrected if necessary.
4.5 Standard stock solution (sulfur content is about 1000mg/L). Add a small amount of solvent to a 100mL volumetric flask, and accurately weigh the sulfur standard substance
(Thiophene is about 0.26g or dibenzothiophene is about 0.58g), accurate to 0.0001g, transferred to a volumetric flask, and diluted to the mark with solvent. Sulfur Standard
The validity period of the quasi-stock solution is three months. The sulfur standard stock solution should be sealed and stored.
4.6 Sulfur series standard solution. The sulfur standard stock solution (4.5) can be diluted to prepare a series of sulfur standard solutions of suitable concentration, in mg/L.
A commercially available certified sulfur standard solution can also be used.
5 Apparatus and equipment
5.1 Burning furnace
Electric heating, the temperature can reach enough to oxidize and burn the sample, and oxidize the sulfur in it to sulfur dioxide.
5.2 Combustion tube
It is made of quartz, and can use quartz tubes with two structures. direct injection mode and boat injection mode. The direct injection method is directly with a syringe
The sample is injected into the high temperature oxidation zone; the boat sampling method is to inject the sample into the sample boat, and use the sampler to push it to the high temperature zone of the sampling tube. Burn
The burner tube should have oxygen and carrier gas inlet branches. The oxidation zone of the combustion tube should be large enough to ensure complete oxidation and combustion of the sample.
5.3 Flow controller
A stable supply of oxygen and carrier gas should be ensured.
5.4 Drying tube
The instrument should be equipped with a membrane drying tube to remove water vapor from the reaction product before it enters the detector.
5.5 UV fluorescence detector
The quantitative detector can measure the fluorescent signal emitted when the excited sulfur dioxide formed after being irradiated by the ultraviolet light source returns to the ground state.
5.6 Syringe
Can choose 100μL, 20μL, 10μL or other suitable volume micro syringe.
5.7 Sampling system
5.7.1 Direct sample injection system. The sampler can inject the sample in the syringe into the carrier gas flow of the combustion tube at a uniform speed, and the vaporized sample is loaded with it.
The gas enters the oxidation zone of the combustion tube.
5.7.2 Boat sampling system. The sampling boat is made of quartz. The sampler can completely push the sample boat into the high temperature zone of the combustion tube, or it can be removed from the combustion tube.
The tube is pulled out. The injection port is equipped with a cooling device. When the injection boat pulled out from the high temperature zone is returned to the injection port, this device can make the injection boat completely cold.
However, the next sample measurement can be performed after cooling. You can choose to place a quartz wool chip on the sample boat to prevent low-boiling samples from before the sample
Volatile.
5.8 Balance (optional)
Sense amount 0.01mg.
6 sampling
Take samples according to the safety and technical requirements specified in GB/T 3723 and GB/T 6680.
7 Measurement procedure
7.1 Instrument preparation
7.1.1 Put the quartz combustion tube into the combustion furnace and connect the carrier gas and reaction gas pipelines.
7.1.2 Turn on the power, turn on the gas source, adjust the furnace temperature, gas flow, sampling speed and other parameters to the conditions recommended by the instrument manual, and press the instrument
Check the air tightness of the gas circuit. After the baseline of the instrument is stable, the sample can be measured.
Note. For high-carbon samples, in order to prevent carbon deposition, the operator can optimize the operating conditions according to the instrument manufacturer's recommendation to improve the repeatability and
stability.
7.2 Drawing the standard curve
7.2.1 Selection of standard curve range and standard solution concentration. use sulfur series standard solution (4.6) as the standard solution for calibration. Against
Different standard curves can be used for samples with the same concentration range. The recommended concentration range of the standard curve is shown in Table 1.Standard curve
The quasi-solution concentration range should include the concentration of the sample to be tested.
7.2.2 Cleaning of the syringe. Before the analysis, rinse the syringe with the standard solution. If there are bubbles in the liquid column, rinse the injection again
And redraw the standard solution.
7.2.3 The pipetting method of the standard solution can be one of the following two methods.
a) Volume method. Take the sample with a syringe and adjust it to the required scale, pull back the plunger of the syringe, and inhale a period of air to make the lowest liquid level
Fall to the 10% mark and record the volume of liquid in the syringe. After the sample is injected, pull the syringe back to make the lowest liquid level drop to 10% of the mark.
Record the volume of liquid in the syringe, and the difference between the two volume readings is the volume of the sample. You can also use a fully automatic sampler for sample injection.
b) Gravimetric method. Use a syringe to extract the sample to the required volume according to the method described in 7.2.2, and weigh the mass of the syringe before and after the sample is injected.
The difference is the quality of the sample.
7.2.4 Establishment of the standard curve. After sampling, use a direct sampling system or a boat sampling system to inject the standard solution in the syringe into the combustion tube
Or in the sample boat, record the response value of sulfide, each sample should be repeated three times, and the relative standard deviation of three repeated determinations should not exceed 5%
(Except blank), and deduct reagent blank. The average value of the response of each standard solution minus the average value of the reagent blank is the average value of the net response.
The sulfur mass (ng) of each standard solution is the abscissa, and the corresponding average value of the net response is the ordinate. Draw a standard curve, which should be linear
Yes, the linear correlation coefficient should be greater than 0.99.Before using the boat sampling system to analyze samples, push the empty boat into the combustion furnace to ensure that the sample boat is
Clean; and the sample can be injected again after the boat is completely cooled.
7.3 Determination of samples
Use a syringe to inject the sample, clean the syringe with the sample to be tested 3 to 5 times, according to the operation method of 7.2.2 to 7.2.4, under the same conditions
Inject the sample into the combustion tube or the sample boat, measure twice in parallel, record the response value of sulfur, and select the standard curve of the appropriate concentration range to calculate
The mass of sulfur in the sample. The sample injection method used for sample determination should be consistent with the sample injection method when the standard curve is established.
8 Result calculation
8.1 Calculation
8.1.1 When the volumetric method is used for sampling, the sulfur content c1 in the sample, in milligrams per liter (mg/L), is calculated according to formula (2).
8.1.2 When the volumetric method is used for sample injection, the sulfur content w in the sample, in milligrams per kilogram (mg/kg), is calculated according to formula (3).
8.1.3 When sampling by gravimetric method, the sulfur content w in the sample, in milligrams per kilogram (mg/kg), is calculated according to formula (4).
8.2 Presentation of results
Take the arithmetic average of two parallel determinations as the analysis result, and round off the value according to GB/T 8170 to the nearest 0.1mg/kg
(Or 0.1mg/L).
9 Precision
9.1 Repeatability
In the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same test object in a short time.
The absolute difference between the two independent test results obtained by independent testing is not greater than the repeatability limit (r) specified in Table 2 to be greater than the repeatability limit
The condition of (r) does not exceed 5%.
9.2 Reproducibility
In different laboratories, different operators operate different equipment, and according to the same test method, the same test object is independently processed.
The absolute difference between the two independent test results obtained by the test is not greater than the reproducibility limit (R) specified in Table 2, to be greater than the reproducibility limit (R)
The condition does not exceed 5% as a prerequisite.
10 Quality Control and Assurance
10.1 Quality control (QC) sample analysis is required before daily sample analysis. This sample can be a certified sulfur standard solution or
Therefore, it is a self-prepared standard solution, or the property is stable, and the actual average value is determined by repeated analysis and mathematical statistics.
sample.
10.2 If a self-prepared standard solution is used to make the standard curve, another quality control sample different from this standard solution should be used to compare the curve.
Line for analysis and verification.
10.3 Quality control samples are required to check the performance of the system every day. If the deviation of the measurement results of the quality control samples is greater than 10%, the system should be checked according to 7.2.
Draw a new standard curve.
11 Report
The report should include the following.
a) All information about the sample, such as name, batch number, sampling location, sampling time, etc.;
b) Number of this part;
c) Measurement results;
d) Details and descriptions of any abnormal phenomena observed in the measurement;
e) The name of the analyst and the date of analysis, etc.;
f) Any operation not included in this section and descriptions of freely selected operating conditions.
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