GB/T 42908-2023 PDF English
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Determination of organic halogen content in textile dyeing and finishing auxiliaries
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GB/T 42908-2023: Determination of organic halogen content in textile dyeing and finishing auxiliaries
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
GB/T 42908-2023
Determination of organic halogen content
in textile dyeing and finishing auxiliaries
ISSUED ON: AUGUST 6, 2023
IMPLEMENTED ON: MARCH 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 ... 4
4 Principle ... 5
5 Reagents or materials ... 5
6 Instruments and equipment ... 6
7 Test steps ... 7
8 Test data processing ... 10
9 Lower limit of determination, recovery rate, and precision ... 10
10 Test report ... 11
Annex A (informative) Purification preparation of activated carbon ... 12
Annex B (informative) Halide ion separation chromatogram ... 13
Determination of organic halogen content
in textile dyeing and finishing auxiliaries
WARNING -- Personnel using this document shall have practical experience in
regular laboratory work. This document does not identify all possible security
issues. Users are responsible for taking appropriate safety and health measures
and ensuring compliance with the conditions specified in relevant national
regulations.
1 Scope
This document describes the method for the determination of organic halogen content
in textile dyeing and finishing auxiliaries.
This document applies to the determination of organic halogen content in various types
of textile dyeing and finishing auxiliaries, including organic fluorine, organic chlorine,
and organic bromine.
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 6682 Water for analytical laboratory use - Specification and test methods
GB/T 8170-2008 Rules of rounding off for numerical values & expression and
judgement of limiting values
3 Terms and definitions
For the purpose of this document, the following term and definition apply.
3.1
organic halogen
Halogens combined with organic compounds.
NOTE 1: The organic halogen compounds in this document include organic compounds of fluorine
(F), chlorine (Cl), and bromine (Br), except iodine (I).
NOTE 2: Under the test conditions of this document, some inorganic halogen compounds will also
be determined as organic halogens if they are not removed from the test.
4 Principle
Disperse or dissolve the sample in a nitric acid aqueous solution, use activated carbon
to adsorb the organic halide in the solution, and put the activated carbon adsorbed with
the organic halide into a high-temperature furnace for combustion, cracking, and
gasification. Its product, hydrogen halide (hydride of fluorine, chlorine, bromine), is
absorbed by alkaline aqueous solution, and then the halogen ions are separated and
determined by ion chromatography and quantified by the external standard method.
5 Reagents or materials
Unless otherwise specified, only use reagents confirmed to be of analytical grade and
first-grade water specified in GB/T 6682. It is recommended that the containers used
be cleaned with nitric acid solution (5.8) before use, and then rinsed with water.
5.1 Activated carbon: granular (0.5 mm ~ 2.5 mm). See Annex A for purification
preparation method.
5.2 Oxygen: purity greater than or equal to 99.995 % (volume fraction).
5.3 Argon gas: purity greater than or equal to 99.99 % (volume fraction).
5.4 Nitric acid.
5.5 Potassium hydroxide, guaranteed reagent.
5.6 Anhydrous sodium carbonate, guaranteed reagent.
5.7 Sodium bicarbonate, guaranteed reagent.
5.8 Nitric acid solution, 1 mol/L: PIPETTE 67 mL of nitric acid (5.4), ADD water to
make the volume to 1000 mL.
5.9 Sodium nitrate solution, 0.85 g/L: WEIGH 17 g of sodium nitrate and DISSOLVE
it in a small amount of water, ADD 1.4 mL of nitric acid (5.4), TRANSFER it to a 1000
mL volumetric flask, and DILUTE to the mark with water. Then use a pipette to transfer
50 mL of the solution, and then dilute to 1000 mL with water.
5.10 Organic halogen reference solutions, 0.25 mg/mL: WEIGH 184.4 mg of 4-
fluorobenzoic acid, 110.3 mg of 4-chlorobenzoic acid, and 62.9 mg of 4-bromobenzoic
acid, ADD water to dissolve respectively and DILUTE to 100 mL to prepare reference
solutions of organic fluorine, organic chlorine and organic bromine with mass
concentrations of 0.25 mg/mL. Dilute as needed when using.
NOTE: Stored in an airtight plastic container at 4 °C, the validity period is 12 months.
5.11 Potassium hydroxide solution, 30 mmol/L: WEIGH 1.68 g of potassium hydroxide
(5.5), DISSOLVE it in water and DILUTE to 1000 mL.
5.12 Mixed solution of 3.2 mmol/L sodium carbonate and 1.0 mmol/L sodium
bicarbonate: WEIGH 0.3392 g of anhydrous sodium carbonate (5.6) and 0.0840 g of
sodium bicarbonate (5.7), DISSOLVE with water and DILUTE to 1000 mL.
5.13 Halogen ion mixed standard stock solution, 1 mg/mL: BAKE the reference
reagents of sodium fluoride, sodium chloride, and sodium bromide at 105 °C for 120
min (or burn at 500 °C for 30 min), COOL and PLACE in a desiccator. WEIGH 2.2105
g of sodium fluoride, 1.6485 g of sodium chloride, and 1.2877g of sodium bromide
after drying, DISSOLVE them in water and DILUTE to 1000 mL. The mass
concentrations of F-, Cl-, and Br- ions in the stock solution are all 1 mg/mL. Or purchase
commercially available standard solutions.
NOTE: Stored in an airtight plastic container at 4 °C, the validity period is 12 months.
5.14 Halogen ion mixed standard working solution: DILUTE the halide ion mixed
standard stock solution (5.13) with water, and prepare halide ion mixed standard
working solution with an appropriate series of concentrations as needed. It is
recommended that the mass concentration of F-, Cl-, and Br- ions be in the range of 0.10
mg/L ~ 2 .00 mg/L.
NOTE: Stored in an airtight plastic container at 4 °C, the validity period is 12 months.
6 Instruments and equipment
6.1 Ion chromatograph: equipped with conductivity detector.
6.2 High-temperature combustion device: It consists of a tube furnace, a cracking tube,
a quartz boat, and a controller. The schematic diagram is shown in Figure 1, or
equivalent. The tube furnace can control the temperature within the range of 500 °C ~
1000 °C, with an error of less than 10 °C.
Halogen-free gloves shall be worn during sample collection, and samples shall be
sealed and stored in polyethylene bags or bottles. If the sample analysis cannot be
completed within 7 days after sampling, it shall be stored frozen to reduce
biodegradation and reduce the loss of volatile halogen compounds.
Take at least 0.5 g of a representative sample, and weigh no less than 2 homogeneous
samples of 10 mg ~ 50 mg (accurate to 0.1 mg).
7.2 Activated carbon adsorption
7.2.1 PUT the weighed sample into a 100 mL Erlenmeyer flask (6.3) with a ground
stopper, ADD 50 mL of sodium nitrate solution (5.9), and ADJUST the pH value to less
than 2 with nitric acid solution (5.8).
7.2.2 ADD 50 mg of activated carbon (5.1) to the Erlenmeyer flask, COVER it with a
ground stopper, PLACE it in the oscillator (6.4) to oscillate and absorb at room
temperature for 12 hours. After adsorption, TRANSFER the solution and activated
carbon to the filtration device (6.5) for filtration, and then WASH the activated carbon
particles several times with 25 mL of sodium nitrate solution (5.9). Then PUT the
activated carbon particles into the quartz boat and proceed with combustion and
cracking according to step 7.3.
7.3 Combustion and cracking
7.3.1 WARM UP the tube furnace in advance, ADJUST the oxygen flow rate to more
than 160 mL/min, and VENTILATE for more than 10 minutes to stabilize the
instrument.
7.3.2 CONNECT the outlet end of the cracking tube to the absorption tube (6.6)
containing 10 mL of potassium hydroxide solution (5.11).
7.3.3 MOVE the quartz boat filled with activated carbon particles to the dry area of the
combustion tube, LET IT STAND for more than 5 minutes. There shall be no water
condensation in the low temperature area of the combustion tube.
7.3.4 PUSH the quartz boat into the high-temperature area of the combustion tube (set
to 950 °C) for full combustion and cracking. The duration shall not be less than 3
minutes.
7.3.5 MOVE the quartz boat to the low temperature area and continue to blow oxygen
for cooling for more than 2 minutes. TAKE OUT the absorption tube, FILTER the
absorption solution through the needle filter head (6.9), for determination.
7.4 Analytical methods
7.4.1 Chromatographic conditions
The best analysis conditions can be selected according to different instruments and
equipment. The reference conditions for chromatographic analysis are as follows.
a) Chromatographic conditions one:
● Chromatographic column: hydroxide selectivity, anion exchange column, 250
mm × 4 mm (inner diameter);
● Column temperature: 30 ℃;
● Eluent: potassium hydroxide solution (5.11);
● Flow rate:1.0 mL/min;
● Sample injection volume: 25 μL.
b) Chromatographic conditions two:
● Chromatographic column: carbonate selectivity, anion exchange column, 150
mm × 4 mm (inner diameter);
● Column temperature: 30 ℃;
● Eluent: a mixed solution of 3.2 mmol/L sodium carbonate and 1.0 mmol/L
sodium bicarbonate (5.12);
● Flow rate: 0.7 mL/min;
● Sample injection volume: 20 μL.
7.4.2 Qualitative analysis
Analyze the halide ion mixed standard working solution (5.14) and absorption solution
(7.3.5) in sequence according to the analysis conditions of 7.4.1, and conduct qualitative
analysis based on the retention time of F-, Cl- or Br- ions. The halide ion separation
chromatogram of the standard working solution is shown in Figure B.1 and Figure B.2
in Annex B.
7.4.3 Quantitative analysis
Plot a standard working curve with the mass concentration of F-, Cl- or Br- ions in the
halide ion mixed standard working solution (5.14) as the abscissa and the corresponding
peak area as the ordinate. According to the chromatographic peak area of F-, Cl- or Br-
ions in the absorption solution (7.3.5), use the external standard method for
quantification. The response value of the target substance in the sample solution shall
be within the linear range of testing of the instrument. If the content exceeds the range
of the standard working curve, the sample solution shall be diluted to an appropriate
concentration before analysis.
The lower limit of determination of organic fluorine, organic chlorine or organic
bromine in this document is 25.0 mg/kg.
9.2 Recovery rate
The standard-adding recovery rates of organic fluorine, organic chlorine or organic
bromine in this document are all 85 % ~ 110 %.
9.3 Precision
The absolute difference between the two independent test results obtained in the same
laboratory, by the same operator using the same equipment, according to the same test
method, by testing the same tested object independently of each other in a short period
of time, is not greater than 10 % of the arithmetic mean of the two measured values,
provided that the case, where it is greater than 10 % of the arithmetic mean of the two
measured values, does not exceed 5 %.
10 Test report
The test report should at least provide the following content:
a) sample source and description;
b) serial number of this document;
c) test conditions;
d) test results;
e) any deviation from the details of this document;
f) test date.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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