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GB/T 40111-2021 (GB/T40111-2021)

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GB/T 40111-2021: PDF in English (GBT 40111-2021)
GB/T 40111-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 75.080
CCS E 30
Standard test method for fluorine, chlorine and sulfur
in petroleum products - Combustion-ion
chromatography
ISSUED ON: MAY 21, 2021
IMPLEMENTED ON: DECEMBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Terms and definitions ... 5 
4 Principle ... 5 
5 Interference ... 5 
6 Instruments and equipment... 5 
7 Reagents and materials ... 10 
8 Sampling ... 11 
9 Preparation ... 12 
10 Calibration ... 13 
11 Test steps ... 15 
12 Result calculation ... 16 
13 Result expression ... 17 
14 Quality control ... 17 
15 Precision and deviation ... 17 
Bibliography ... 19 
Standard test method for fluorine, chlorine and sulfur
in petroleum products - Combustion-ion
chromatography
Warning -- The personnel using this document should have practical
experience in formal laboratory work. The use of this document may
involve certain hazardous materials, equipment and operations. This
document does not point out all possible safety issues. The user is
responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions stipulated by relevant national
laws and regulations.
1 Scope
This Standard specifies the test method that uses combustion-ion
chromatography to determine fluorine, chlorine and sulfur content in petroleum
products, interference, instruments and equipment, reagents and materials,
sampling, preparation, calibration, test procedures, calculation of results,
expression of results, as well as precision and deviation.
This Standard is applicable to the determination of fluorine, chlorine and sulfur
content in petroleum products of which the boiling point range is 30°C~380°C
and the determination range is 0.30mg/kg~15.00mg/kg, including gasoline,
ethanol gasoline, naphtha, distillate, jet fuel, diesel, biodiesel blended fuel. This
method can be also used for the samples outside this range, but the precision
has not been determined.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 1884, Petroleum and liquid petroleum product - Determination of
density - Hydrometer method
GB/T 1885, Petroleum measurement tables
GB/T 4756, Method for manual sampling of petroleum liquids
6.2.7 Humidification device: a certain flow rate of primary water (7.1) can be
passed into the high-temperature combustion tube to obtain a high-temperature
hydrolysis environment.
6.3 Absorption unit
6.3.1 Connecting pipe: It is used to connect the high-temperature combustion
pipe and the absorption pipe. There shall be pipelines for the water inlet and
the water outlet. After the specimen is completely burned in the high-
temperature combustion tube, the instrument automatically flushes the
connecting pipe with grade one water (7.1) and transfers all to the absorption
pipe (6.3.2).
6.3.2 Absorption tube: At least containing 10mL of absorption solution. During
the sample combustion process, the absorption liquid in the tube continuously
absorbs gas and all liquids to ensure that all combustion products (HX and SOx)
are absorbed. After the combustion is over, the volume can be automatically
adjusted to the required volume. A quantitative absorption solution can be
automatically injected into the ion chromatography instrument through the
quantitative loop.
6.3.3 After the absorption liquid is injected into the ion chromatography
instrument, and before the next specimen is burned, use grade one water (7.1)
to rinse the connecting tube and absorption tube, so as to minimize the
contamination of the previous sample.
6.4 Ion chromatography unit
6.4.1 Pump: transport eluent.
6.4.2 Continuous eluent generator (optional): the device that can automatically
prepare and purify eluent, including electrolytic eluent generator method and
automatic quantitative tube method. Without reducing the precision and
accuracy of the method, other continuous eluent generators can be used.
6.4.3 Anion pre-concentration column (optional): mainly play a role in pre-
concentrating anions and eliminating matrix effect. If a pre-concentration
column is installed, then the remaining hydrogen peroxide can be removed
before the absorption liquid is injected into the guard column and the separation
column, so as to eliminate the potential interference to the fluoride ion
chromatographic peak resolution.
6.4.4 Guard column: protect the separation column from contamination by
strongly retained components. At the same time, a better separation effect can
be obtained.
6.4.5 Separation column: anion exchange column, which can make the anion
7.11 Absorbent: Take 0.7mL of 30% hydrogen peroxide (7.7) in a 2000mL
volumetric flask. Use grade one water (7.1) to dilute to the scale mark. The
purpose of adding hydrogen peroxide to the absorption solution is to convert all
the SOx in the gas to be measured into SO42-. If the sulfur content in the sample
is not determined, hydrogen peroxide cannot be added to the absorption
solution. Use grade one water (7.1) as absorbent.
NOTE 1: Under the premise of meeting the precision of the method, other concentrations
of absorbents can also be used.
NOTE 2: When the sulfur content in the sample is less than 15mg/kg, hydrogen peroxide
may not be added. Select according to the determination situation of the instrument. When
the difference in the area count of the sulfur peak obtained with and without hydrogen
peroxide in the absorbent is less than 5%, hydrogen peroxide may not be added to the
absorbent.
7.12 Quality control (QC) samples: stable, representative samples or use
standard working solutions (9.2.2), used to verify the accuracy of the entire test
process, see Chapter 14.
7.13 Quartz wool.
7.14 Carrier gas: argon or helium, with a purity of not less than 99.99%.
NOTE: Purification device can be used to remove impurities, such as: molecular sieve to
remove moisture. Use activated carbon or other materials with the same function to adsorb
hydrocarbon compounds.
7.15 Oxygen: used as combustion gas, with a purity of not less than 99.75%.
7.16 Nitrogen (optional): access to the eluent tank to prevent air from entering
or generating bubbles. The purity is not less than 99.99%.
8 Sampling
8.1 Conduct sampling according to GB/T 4756 and GB/T 27867 methods.
Samples containing volatile components shall be opened before the
determination of the sample container. The samples shall be analyzed as soon
as possible after taking out the samples to avoid the loss and contamination of
the measured elements.
8.2 After the sample is collected in the container, if it is not used immediately,
the sample shall be thoroughly mixed in the container before analysis.
NOTE: Because there are light components in the sample, pay attention to safety when
mixing.
and burned. If carbon deposits are found in the sample boat, the residence time
of the sample boat in the combustion furnace shall be increased. If carbon
deposits are found at the end of the high-temperature combustion tube, slow
down the sampling speed of the sample boat or increase the residence time of
the sample boat at the front end of the high-temperature combustion tube. It
can also take these two measures at the same time. Remove the carbon
deposits on the parts according to the requirements of the instrument manual.
Reassemble the instrument.
10.5 After the standard working solution analysis is completed, the sample boat
is pulled back to the refrigeration module (6.2.3). The sample boat shall stay on
the refrigeration module for at least 100s, or longer. Allow the sample boat to
cool down completely. Then proceed to the next standard working solution test.
11 Test steps
11.1 Prepare samples according to Chapter 8.
11.2 Use a syringe to inject a quantitative sample, such as 100μL, into the
sample boat. According to the determination conditions of the analytical
standard working solution, determine the specimen in the same way to get the
chromatogram of the specimen. Integrate the chromatographic peaks of
fluorine, chlorine and sulfur elements to obtain the chromatographic peak area
of each element. In order to reduce the errors caused by combustion efficiency
and absorption efficiency, the conditions of the specimen analysis shall be
consistent with the conditions of the analysis standard working solution.
11.3 After analyzing the specimen, check the high-temperature combustion
tube and the various components in the flow path through which the gas passes
for carbon deposits to ensure that the specimen is completely oxidized and
burned. If carbon deposits are found in the sample boat, the residence time of
the sample boat in the combustion furnace shall be increased. If carbon
deposits are found at the end of the high-temperature combustion tube, slow
down the sampling speed of the sample boat or increase the residence time of
the sample boat at the front end of the high-temperature combustion tube. It
can also take these two measures at the same time. Remove the carbon
deposits on the parts according to the requirements of the instrument manual.
Reassemble the instrument.
11.4 After the sample analysis is completed, the sample boat is pulled back to
the refrigeration module (6.2.3). The sample boat shall stay on the refrigeration
module for at least 100s, or longer. After the sample boat can be completely
cooled, proceed to the next specimen test. This step is especially important for
specimens with a low initial boiling point.
(g/cm3).
13 Result expression
Take the arithmetic average of the two repeated determinations as the
determination result, in milligrams per kilogram (mg/kg). The result is retained
to 0.01mg/kg.
14 Quality control
14.1 After each startup, the QC sample (7.12) shall be determined at least once
before analysis.
14.2 If the laboratory has established quality control and quality assurance
procedures, it can be used to confirm the reliability of the determination results.
14.3 If the laboratory has not established quality control and quality assurance
procedures, it can refer to NB/SH/T 0843 as the evaluation system.
15 Precision and deviation
15.1 Precision
15.1.1 Overview
The precision is obtained through collaborative experiments conducted by 6
laboratories on 22 samples, including: gasoline, ethanol gasoline, diesel,
naphtha, distillate oil, jet fuel, diesel, biodiesel blended fuel. Refer to GB/T 6683
to determine it through statistical analysis results between laboratories. Judge
the reliability of the test results according to 15.1.2 and 15.1.3 (95% confidence
level).
NOTE: If the specimens containing volatile components are not properly stored, it will affect
the measurement results.
15.1.2 Repeatability (r)
The same operator, in the same laboratory, uses the same instrument to
continuously measure the same specimen. The difference between the two test
results shall not exceed the repeatability limit of the method in Table 3. See
Table 4 for typical repeatability values of samples at different concentrations.
15.1.3 Reproducibility (R)
......
 
(Above excerpt was released on 2021-07-30, modified on 2021-07-30, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT40111-2021