NBSHT6044-2021 PDF English
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| NB/SH/T 6044-2021 | English | 170 |
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Standard test method for determining the biobased content of liquid petroleum products using radiocarbon analysis by accelerator mass spectrometry
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Similar standards NB/T 10077 NBSHT6044-2021: (Determination of Bio-based Content of Radiocarbon in Liquid Petroleum Products Accelerator Mass Spectrometry)
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SH
PETROCHEMICAL INDUSTRY STANDARD
ICS 75.080
CCS E 30
Standard test method for determining the biobased content
of liquid petroleum products using radiocarbon analysis by
accelerator mass spectrometry
Issued on: NOVEMBER 16, 2021
Implemented on: MAY 16, 2022
Issued by. National Energy Administration
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 5
3 Terms and definitions... 5
4 Method overview... 7
5 Application of the method... 7
6 Safety considerations... 9
7 Instrumentation... 9
8 Reagents and materials... 10
9 Sampling... 10
10 Preparation of graphitized specimens... 10
11 Test steps... 12
12 Calibration... 12
13 Calculation... 13
14 Presentation and interpretation of results... 14
15 Precision and deviation... 16
16 Report... 16
Appendix A (Informative) Example of specimen graphitization apparatus... 18
Standard test method for determining the biobased content
of liquid petroleum products using radiocarbon analysis by
accelerator mass spectrometry
Warning. The use of this document may involve certain hazardous materials,
operations, equipment; however, it does not address all safety concerns. Therefore,
users shall establish appropriate safety precautions and determine the
applicability of relevant regulatory restrictions before using this document.
1 Scope
This document specifies a method for determining the biobased content of liquid
petroleum products by radiocarbon analysis using accelerator mass spectrometry.
This document applies to organic liquid petroleum products containing carbon-based
components that produce carbon dioxide (CO2) gas when burned in the presence of
oxygen.
Caution. This document is intended for use in laboratories that are not exposed to
artificial 14C. Artificial 14C is commonly used in biomedical research in accelerator
mass spectrometry (AMS) laboratories, where biobased materials can be present
at concentrations exceeding 1000 or 100% and 100000 times greater than 1%
biobased material. Artificial 14C can be ubiquitous on laboratory door handles,
pens, desks, other surfaces, potentially contaminating samples and producing
falsely high biobased content results. Isolation has been shown to be the only
effective method to prevent contamination. Laboratories exposed to artificial 14C
require a completely independent chemistry laboratory and rigorous testing and
validation procedures. Acceptable conditions include the following.
a) Disclosure to clients that the laboratory whose samples are being tested also
handles 14C;
b) The chemistry laboratories handling 14C and testing biobased carbon
samples are located in different buildings;
c) Separate testing personnel and no access to each other's buildings;
d) No shared common areas such as lunchrooms and offices;
e) No sharing of supplies or chemicals;
f) Quasi-simultaneous quality assurance measurements are performed on the
detectors to ensure that the detectors themselves are not contaminated.
2 Normative references
The contents of the following documents, through normative references, constitute
essential provisions of this document. For dated references, only the edition
corresponding to that date applies to this document. For undated references, the latest
edition (including all amendments) applies to this document.
GB/T 4756 Method for manual sampling of petroleum liquids
NB/SH/T 0656 Determination of carbon, hydrogen and nitrogen in petroleum
products and lubricants - Elemental analyzer method
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Radiocarbon 14C
A radioactive isotope of carbon, namely carbon-14 (14C); the nucleus of carbon-14
consists of 6 protons and 8 neutrons.
Note. 14C is produced by cosmic rays striking nitrogen atoms in the air. Its half-life is
approximately 5730 years ± 40 years. On earth, 99% of carbon exists as 12C, approximately
1% as 13C, only one part per trillion (0.0000000001%) is 14C, presenting in the atmosphere.
3.2
Half-life
The time required for half of the nuclei of a radioactive element to decay. The half-
life of 14C is approximately 5730 ± 40 years.
3.3
Fossil carbon
Carbon which is essentially free of radioactive 14C, because its age is much greater
than the half-life of 14C.
3.4
Modern carbon
Organic carbon content
The mass percentage of organic carbon in a sample relative to the total mass of the
sample.
3.11
Biobased carbon content on mass basis
The percentage of mass of biobased carbon in a sample to the total mass of the
sample.
3.12
Accelerator mass spectrometry (AMS)
An ultrasensitive technique used to measure naturally occurring radionuclides. In
AMS, atoms are ionized and accelerated to high energies; separated based on
momentum, charge, mass; counted individually in a Faraday collector or solid-state
or gas detector. This high-energy separation is very effective in filtering out isobaric
interferences, allowing AMS to accurately measure the abundance ratio of 14C/12C
to the order of 10⁻¹⁵. At this level, the uncertainty is based on the statistics of a
Poisson distribution.
4 Method overview
Carbon-based components in a specimen are burned to CO2 in a high-temperature
oxygen environment. The CO2 is then purified, dehydrated, collected, reduced to
graphite. The 14C/12C ratio in graphite is measured using accelerator mass spectrometry
(AMS) and compared to international radiocarbon reference materials, to obtain the
percentage modern carbon (pMC) or fraction modern carbon (fM). The pMC is divided
by the atmospheric correction factor (REF) used at the time of specimen measurement,
to determine the specimen's biobased carbon content.
5 Application of the method
5.1 This document provides a method for accurately determining the biobased carbon
content of liquid petroleum products derived from living organisms. Carbon in living
organisms (such as crops or plants growing in nature) exchanges in equilibrium with
atmospheric CO2 until respiration or metabolism ceases. When applying this test
method, special consideration shall be given to samples from artificial environments;
samples that have absorbed CO2 from artificial environments are not within the scope
of this method.
5.2 This method can directly distinguish between carbon derived from biomass and
carbon derived from fossil fuels, for example, distinguishing between biofuel ethanol
derived from biomass such as corn and sorghum and coal-based ethanol derived from
fossil fuels such as coal. This document can be used to quantify the biofuel content in
fossil fuels, for example, by measuring the amount of biofuel ethanol added to ethanol
gasoline and the amount of biobased additives added to aviation fuel. This document
can provide testing methods for the promotion and implementation of products
containing biofuels, such as ethanol gasoline.
5.3 This document does not consider the sample's inherent properties, function,
geographic origin, or environmental influences.
5.4 All laboratories implementing this document shall properly use international
standard reference materials, to ensure the traceability of carbon isotope determinations
and the validity of the stated uncertainties. The primary international standard reference
materials for 14C are NIST SRM 4990B (designated as OXI, HOxI, Oxalic acid I) or
NIST SRM 4990C (designated as OXII, HOxII, Oxalic acid II). The fM value for NIST
SRM 4990B is 1.0398; the fM value for NIST SRM 4990C is 1.3407.
5.5 The 14C/12C isotope ratio of the sample is measured, using accelerator mass
spectrometry (AMS). The 14C/12C isotope ratio of the sample is compared to the 13C/12C
isotope ratio of an international standard radiocarbon reference material (NIST SRM
4990B or NIST SRM 4990C), then corrected using the ratio of the stable isotopes
13C/12C. This yields the percentage modern carbon (pMC) or the fraction modern carbon
(fM) of the sample.
5.6 The pMC value measured by accelerator mass spectrometry (AMS) shall be
corrected using the ratio of the stable isotopes 13C/12C. Whenever possible, the ¹³C/¹²C
value measured within the AMS should be used for correction. If the instrument cannot
measure the 13C/12C value, calibration shall be performed using δ13C measured by
IRMS (stable isotope mass spectrometry), CRDS (cavity ring-down spectroscopy
isotope carbon analyzer), or other equivalent techniques that provide a measurement
accuracy within ±0.3‰. For δ13C measurements, standard materials shall be NIST SRM
8539, NIST SRM 8540, NIST SRM 8541, NIST SRM 8542, or other equivalent
materials traceable to Vienna Pee Dee Belemite (VPDB).
5.7 The accelerator mass spectrometer used in this document has a measurement error
of 0.1% ~ 0.5% (1 RSD) and a relative standard deviation of 0.1 pMC ~ 0.4 pMC.
However, comparative experiments have found that the total uncertainty of biobased
carbon content measured by different laboratories can reach ±3% (absolute value). This
error does not include uncertain sources of error due to biological sources.
5.8 Unless otherwise specified, the error in this method for determining the percentage
of modern carbon in international standard reference materials shall not exceed ±5% of
the certified value.
6 Safety considerations
6.1 This document does not address specific safety and regulatory requirements related
to radioactivity, sample preparation, instrument operation. Users of this document are
responsible for establishing appropriate safety and health practices. When
implementing this document, users shall also comply with relevant Chinese regulations,
particularly those related to the use of open radioactive sources. Although 14C is one of
the safest isotopes, relevant Chinese regulations shall be followed when implementing
the methods in this document.
6.2 Glass and metal used must withstand temperatures exceeding 900 °C in a closed
oxygen-containing system; failure to do so may pose a safety hazard. Operators shall
avoid implosion/explosion of glass tubes. Laboratory safety precautions shall always
be observed, with particular attention to eye, respiratory, skin protection.
7 Instrumentation
7.1 Accelerator mass spectrometer. Determine the ratio of 14C/12C in a sample with an
instrumental measurement error of 0.1% ~ 0.5% (1RSD). Details regarding instrument
operation shall be obtained from the instrument manufacturer.
7.2 Vacuum manifold system. A device that combusts samples into CO2 and purifies
and collects the resulting gas. It has gas lines for exhausting air and non-condensable
gases; functions for introducing samples, distilling water, transferring cryogenic gases,
monitoring temperature and pressure. This device is used to quantitatively combust
carbon-based components in samples of varying complexity. This document
recommends the device shown in Figure A.1 in Appendix A. However, other devices
with continuous flow interfaces and CO2 capture capabilities are also suitable, provided
that a CO2 recovery rate of 100% ± 5% can be achieved. This apparatus requires the
following components, with appropriate weld fittings used to assemble the components.
a) Fragile seal tube, see Figure A.2 in Appendix A;
b) Flexible fracture tube, see Figure A.2 in Appendix A;
c) A vacuum pump capable of achieving a vacuum of 101 Pa or less;
d) A pressure sensor with a coupled or integrated signal-responsive controller;
e) A CO2 calibration chamber with a volume scale and temperature readout, see
Figure A.2 in Appendix A;
f) Clean quartz tubing for sample combustion and gas transfer, dosing, storage;
g) A hydrogen/oxygen torch or other heating device and/or a gas torch for sealing
the quartz tubing.
7.3 CO2 reduction system to graphite. An apparatus for reducing CO2 to graphite. The
reduction process must prevent contamination with CO2 from the air and loss of CO2
from the sample. This process shall be performed in an enclosed space.
7.4 Temperature-controlled furnace. Capable of reaching 950 °C.
7.5 Analytical balance. Sensitivity 0.00001 g.
8 Reagents and materials
8.1 Dehydrating agent. A slurry mixture of dry ice (frozen solid CO2) and ethanol at -
76 °C, or other material capable of separating water from CO2 in the CO2 collector.
8.2 International standard reference material for radiocarbon. NIST SRM 4990B or
NIST SRM 4990C.
8.3 Note. Available from the National Institute of Standards and Technology (NIST) in
the United States and also from the Atomic Energy Agency (IAEA) in Vienna, Austria.
8.4 Oxygen source. High-purity oxygen, ≥ 99.999% purity, or solid copper oxide (CuO).
8.5 Silver. For halide removal.
8.6 Liquid nitrogen.
8.7 Iron, cobalt, or other catalyst for the reduction of CO2 to graphite.
8.8 Hydrogen. Purity ≥ 99.9%.
9 Sampling
Representative samples shall be collected in accordance with the provisions of GB/T
4756.
10 Preparation of graphitized specimens
10.1 The specimen preparation procedures described in this document utilize a
commonly used method for quantitatively combusting carbon components in specimen
matrices of varying complexity. While this preparation procedure is recommended,
other equipment with continuous flow interfaces and CO2 capture capabilities is also
suitable, provided that a CO2 recovery rate of 100% ± 5% can be achieved.
10.2 Weigh a sufficient amount of specimen. Calculations indicate that the carbon
content of the CO2 recovered after sample combustion shall be 1 mg ~ 10 mg. Place the
weighed specimen in a pre-cleaned quartz tube that has been baked at 900 °C for at
least 2 h and sealed at one end. A quartz tube with an outer diameter of 2 mm and an
inner diameter of 1 mm is typically used. Any quartz tube size that can accommodate a
sufficient specimen is acceptable.
10.3 Then transfer the weighed quartz tube containing the test specimen to another
quartz tube of appropriate size, typically 6 mm outer diameter and 4 mm inner diameter.
10.4 Then connect the above quartz tubes to the vacuum manifold and evacuate to 101
Pa or less.
10.5 If the test specimen is volatile or contains volatile components, first freeze the test
specimen in the quartz tube to -196 °C with liquid nitrogen before evacuating the tube.
After evacuating the tube, seal the quartz tube containing the test sample and then burn
the test specimen in the sealed quartz tube in a 900 °C temperature-controlled furnace
for 2 ~ 4 hours, to convert it to CO2.
10.6 After combustion, score the quartz tube containing the CO2 to create a breakable
seal that will break cleanly within the flexible break tube in the vacuum manifold
system (see Appendix A, Figure A.2).
10.7 The breakable sealed tube containing CO2 is broken within the flexible break tube
in the vacuum manifold system, releasing the CO2 into a CO2 collector, which is
connected to the vacuum manifold (see Appendix A, Figure A.2), where it is rapidly
frozen by cryogenic liquid nitrogen.
10.8 A desiccant is used to distill and separate the water and CO2 in the CO2 collector.
The water is condensed in the sample collector, whilst the CO2 sublimates into a gas
and is transferred to a CO2 calibration chamber at another port on the vacuum manifold
(see Appendix A, Figure A.2) for condensation.
10.9 After all the CO2 has been transferred, close the CO2 calibration chamber and allow
the CO2 to equilibrate to room temperature.
10.10 Use the ideal gas law to calculate the CO2 recovery rate.
10.11 Release the CO2 from the CO2 calibration chamber into the graphitization system
to reduce the CO2 to graphite.
10.12 The process of converting CO2 gas to graphite requires the use of an iron or cobalt
catalyst and the reduction is carried out according to formulas (1) and (2).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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