GB/T 44242-2024 PDF English
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Hydrogen for proton exchange membrane fuel cell vehicles - Determination of inorganic halogenated compounds and formic acid - Ion chromatography method
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GB/T 44242-2024: Hydrogen for proton exchange membrane fuel cell vehicles - Determination of inorganic halogenated compounds and formic acid - Ion chromatography method
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 27.010
CCS F 19
Hydrogen for proton exchange membrane fuel cell vehicles -
- Determination of inorganic halogenated compounds and
formic acid - Ion chromatography method
Issued on: JULY 24, 2024
Implemented on: NOVEMBER 01, 2024
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 Reagents and materials... 5
6 Instruments and equipment... 7
7 Test procedures... 7
8 Test data processing... 10
9 Precision... 11
10 Quality assurance and control... 12
11 Test report... 13
Annex A (informative) Ion chromatography operating conditions and eluent elution
procedures, standard chromatograms and calibration curves... 14
Bibliography... 16
Hydrogen for proton exchange membrane fuel cell vehicles -
- Determination of inorganic halogenated compounds and
formic acid - Ion chromatography method
WARNING -- Hydrogen is a flammable and explosive gas. This document does not
cover all safety issues related to its application. Before using this document, the
user is responsible for formulating appropriate safety and protection measures,
clarifying its limited scope of application, and ensuring compliance with relevant
national laws and regulations and mandatory national standards.
1 Scope
This document describes the principle, reagents and materials, instruments and
equipment, test procedures, test data processing, precision, quality assurance and
control, and test report for the determination of inorganic halogenated compounds and
formic acid in hydrogen for proton exchange membrane fuel cell vehicles by ion
chromatography.
This document is applicable to the determination of inorganic halogenated compounds
and formic acid in hydrogen for proton exchange membrane fuel cell vehicles. The
determination of inorganic halogenated compounds and formic acid in hydrogen for
other purposes shall be carried out in reference. The determination range of inorganic
halogenated compounds and formic acid in hydrogen is 0.025 μmol/mol~0.5 μmol/mol.
The detection limits of hydrogen chloride, chlorine, hydrogen bromide and formic acid
components in hydrogen are 0.014 μmol/mol, 0.007 μmol/mol, 0.002 μmol/mol and
0.001 μmol/mol, respectively.
NOTE. Inorganic halogenated compounds in this document refer to hydrogen chloride, chlorine
and hydrogen bromide which may be present in hydrogen gas.
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 629, Chemical reagent. Sodium hydroxide
GB/T 637, Chemical reagent -- Sodium thiosulfate pentahydrate
GB/T 639, Chemical reagent -- Sodium carbonate anhydrous
GB/T 640, Chemical reagent -- Sodium hydrogen carbonate
GB/T 6682, Water for analytical laboratory use -- Specification and test methods
GB/T 14666, Terms for analytical chemistry
GB/T 43306, Gas analysis -- Sampling guidelines
GB/T 44262, Technical requirements for sampling of hydrogen for proton exchange
membrane fuel cell vehicles
JJF 1342, General Requirements for the Competence of Reference Material
Producers
JJG 823, Ion Chromatographs
3 Terms and definitions
For the purposes of this document, the terms and definitions defined in GB/T 14666
apply.
4 Principle
Inorganic halogenated compounds and formic acid in the hydrogen sample are absorbed
by the alkaline solution to generate halide ions and formate ions. They are separated by
anion chromatography column and detected by conductivity detector. They are
qualitatively determined by retention time and quantitatively determined by calibration
curve.
5 Reagents and materials
5.1 Test water
It shall comply with the requirements of GB/T 6682 for Grade 1 reagent water.
5.2 Reagents
5.2.1 Sodium thiosulfate pentahydrate (Na2S2O3·5H2O). in accordance with the
requirements of GB/T 637 for guaranteed reagents.
5.2.2 Sodium hydroxide (NaOH). in accordance with the requirements of GB/T 629 for
guaranteed reagents.
5.2.3 Sodium carbonate (Na2CO3). in accordance with the requirements of GB/T 639
for guaranteed reagents.
5.2.4 Sodium bicarbonate (NaHCO3). in accordance with the requirements of GB/T 640
for guaranteed reagents.
5.3 Solutions
5.3.1 Chloride stock solution. an aqueous solution with a chloride ion concentration of
1000 mg/L. A commercially available certified standard solution may be selected.
5.3.2 Bromide stock solution. aqueous solution with a bromide ion mass concentration
of 1000 mg/L. A commercially available certified standard solution may be selected.
5.3.3 Formic acid stock solution. aqueous solution with a formate ion mass
concentration of 1000 mg/L. A commercially available certified standard solution may
be selected.
5.3.4 Alkaline solution. aqueous solution with NaOH and S2O32- mass concentrations
of 200 mg/L and 5 mg/L respectively. Accurately weigh 0.200 g of sodium hydroxide
and 0.011 g of sodium thiosulfate pentahydrate and dissolve in appropriate amount of
water. Transfer to a 1000 mL volumetric flask. Add water to the set volume and mix.
Prepare when needed.
5.3.5 Hydroxide eluent. generated online by an automatic eluent electrolytic generator.
5.3.6 Carbonate eluent. aqueous solution with Na2CO3 and NaHCO3 concentrations of
5.0 mmol/L and 0.2 mmol/L respectively. Accurately weigh 0.530 g of sodium
carbonate and 0.017 g of sodium bicarbonate. Dissolve in an appropriate amount of
water. Transfer to a 1000 mL volumetric flask. Add water to the set volume and mix
well.
5.4 Gas reference materials
5.4.1 The qualifications of the research and development (production) institutions of
gas reference materials shall comply with the requirements of JJF 1342.Users shall
give priority to the use of certified gas reference materials.
5.4.2 Hydrogen chloride gas standard substance. hydrogen chloride content is 0.05
μmol/mol. The balance gas is nitrogen or hydrogen. It can be prepared by diluting high-
concentration gas reference material with a gas diluter.
5.4.3 Formic acid gas standard substance. formic acid content is 0.1 μmol/mol. The
balance gas is nitrogen or hydrogen. It can be prepared by diluting high-concentration
gas reference material with a gas diluter.
6 Instruments and equipment
6.1 Instruments
6.1.1 Ion chromatograph. equipped with conductivity detector and anion suppressor.
The main performance indicators of the conductivity detector shall meet the
requirements of JJG 823.It is equipped with anion chromatographic column. The
matrix is divinylbenzene/ethylvinylbenzene polymer or styrene/divinylbenzene
polymer or polyvinyl alcohol. It is with quaternary ammonium functional group, or
other equivalent anion chromatographic columns. The separation degree of the target
ion is not less than 1.5.
6.1.2 Gas diluter. dilution ratio is 20 to 400 times. All pipeline inner walls and
connecting parts must be inertized. Gas diluter shall be calibrated regularly by a
qualified metrology agency.
6.1.3 Balance. the graduation value is 0.0001 g. The balance shall be calibrated
regularly by a qualified metrology agency.
6.2 Equipment
6.2.1 Water purifier. water treatment equipment capable of producing water that meets
the requirements of test water (5.1).
6.2.2 Connecting pipe. polytetrafluoroethylene hose or silicone rubber tube lined with
polytetrafluoroethylene film.
6.2.3 Impact absorption bottle. capacity is 25 mL. Accurate to 0.1 mL. Material can be
glass. Polytetrafluoroethylene material must be tested. The impact absorption bottle
filled with 10 mL of water is left to stand for 4 h. The measured values of the target ions
shall be less than 0.1 mg/L.
6.2.4 Flow meter. range is 1 L/min. Flow rate relative deviation is ≤ 1%.
6.2.5 Volumetric flask. capacity is 100 mL, 1000 mL.
6.2.6 Graduated pipette. capacity is 2 mL, 5 mL, 10 mL.
6.2.7 Sampling gas cylinder. comply with the requirements of GB/T 44262 and GB/T
43306.
7 Test procedures
7.1 Sampling
The sampling of hydrogen for proton exchange membrane fuel cells shall comply with
Prepare calibration samples suitable for testing the content of inorganic halogenated
compounds in hydrogen not greater than 0.07 μmol/mol and the content of formic acid
not greater than 0.05 μmol/mol. Pipette 1 mL of the chloride stock solution (5.3.1),
bromide stock solution (5.3.2) and formic acid stock solution (5.3.3). Place them in a
100 mL volumetric flask. Add water to the set volume and mix well to obtain a mixed
solution with a target ion mass concentration of 10 mg/L. Pipette 0 mL, 2 mL, 4 mL, 6
mL, 8 mL, and 10 mL of the above mixed solutions respectively. Place them in a group
of 100 mL volumetric flasks. Add water to the set volume and mix well to obtain
calibration samples with theoretical mass concentrations of 0 mg/L, 0.2 mg/L, 0.4 mg/L,
0.6 mg/L, 0.8 mg/L, and 1.0 mg/L, respectively.
7.2.5 Preparation of blank samples
Take an impact absorption bottle from the same batch containing 10 mL of absorption
liquid. Disconnect it from the gas source. Shake well for testing.
7.3 Instrument preparation
Optimize the ion chromatography operating conditions and eluent elution procedure
according to the composition of the sample to be tested, the instrument model and
configuration. See Table A.1 in Annex A for typical ion chromatography operating
conditions. See Table A.2 for typical eluent elution procedures.
7.4 Establishment of calibration curve
Inject the calibration samples from low concentration to high concentration in sequence.
Draw the calibration curve with the mass concentration (mg/L) of the target ion as the
horizontal axis and the peak height or peak area as the vertical axis. The typical
chromatogram of the target ion is shown in Figure A.1.The calibration curve of the
target ion is shown in Figure A.2.The calibration curve shall be linear, with R2 ≥ 0.999.
7.5 Blank determination
Inject the blank sample into the ion chromatograph. Determine the content of the target
ions under the same chromatographic conditions as those used to draw the calibration
curve. The measured values of the three target ions in the blank sample shall all be
lower than 0.1 mg/L.
7.6 Specimen measurement
Inject the sample to be tested into the ion chromatograph. Determine the target ion
content under the same chromatographic conditions as those used to draw the
calibration curve. When the target ion content in the sample exceeds the upper limit of
the calibration curve drawing range, dilute with water and re-measure. The target ion
content in the second absorption bottle shall be less than 25% of that in the first
absorption bottle. The sample shall be measured within 7 d after collection.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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