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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Petroleum and Chemical Industry Association.
This standard is under the jurisdiction of SAC/TC 134 Technical Committee on Dyestuff of Standardization Administration of China.
Determination of short chain chlorinated paraffins in textiles dyeing and finishing auxiliaries
Warning: the personnel using this standard shall have practical experience in standard laboratory work. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the theory, reagents and materials, instruments and apparatuses, determination procedures, blank test, test data processing, determination lower limit, recovery rate, precision and test report for the determination of short chain chlorinated paraffins in textiles dyeing and finishing auxiliaries.
This standard is applicable to the determination for the content of short chain chlorinated paraffins (C10~C13) in textiles dyeing and finishing auxiliaries.
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 6682-2008, ISO 3696: 1987, MOD)
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgment of limiting values
3 Theory
Extract the specimen with n-hexane by vibration, then purify the extracted solution and dilute it to a constant volume; dechlorinate the solution via palladium catalysis to convert the short chain chlorinated paraffins into a C10~C13 n-alkane, then inspect it with gas chromatograph which is equipped with a flame ionization detector (GC-FID), and then quantify it by external standard method using the short chain chlorinated paraffin standards with the chlorine content of 55.5% (mass fraction). Where necessary, gas chromatographs equipped with electron capture detector (GC-ECD) or gas chromatograph-mass spectrometer with negative chemical ionization (GC-NCI-MS) shall be used for qualitative confirmation.
4 Reagents and materials
Unless otherwise specified, only recognized analytically pure reagents and Grade-III water (specified in GB/T 6682) shall be adopted.
4.1 Ammonia: 25%~28% (mass fraction).
4.2 Acetic acid: about 36% (mass fraction).
4.3 n-hexane.
4.4 Dichloromethane.
4.5 Cyclopentane.
4.6 Palladium chloride.
4.7 Calcium carbonate.
4.8 Concentrated sulfuric acid: about 98% (mass fraction).
4.9 Elution solution: the volume ratio of n-hexane (4.3) to dichloromethane (4.4) is 1:1.
4.10 Short chain chlorinated paraffin (CAS No.: 85535-84-8) standard: concentration: 100μg/mL; average degree of chlorination: 55.5% (mass fraction).
4.11 Short chain chlorinated paraffin standard working solution: pipette an appropriate amount of short chain chlorinated paraffin standard (4.10), and dilute it with n-hexane (4.3) to prepare the working solution with the concentration of 10.0μg/mL.
4.12 C10, C11, C12 and C13 n-alkane (CAS No.: 124-18-5, 1120-21-4, 112-40-3 and 629-50-5) standards: with the purity greater than 99.5% (mass fraction).
4.13 Acetic acid solution, 5% (mass fraction): pipette 14 mL of acetic acid (4.2) and put it into a 100-mL volumetric flask, and dilute it to the scale with water and shake it well.
4.14 Mixed standard stock solution: respectively weigh an appropriate amount of C10, C11, C12 and C13 n-alkane standard (4.12), and prepare it to the single standard stock solutions (1,000μg/mL) with n-hexane (4.3). Then pipet 10 mL of C10, C11, C12 and C13 single standard stock solutions respectively into a 100-mL volumetric flask and dilute to scale with n-hexane (4.3) to obtain the mixed standard stock solution (100μg/mL).
Note: The standard stock solutions shall be stored at 0℃~4℃ for a validity period of 12 months.
4.15 Mixed standard working solution: respectively pipette an appropriate amount of n-alkane mixed standard stock solution (4.14), and dilute it with n-hexane (4.3) to prepare it to the mixed standard working solutions with the concentrations of 0.5μg/mL, 1.0μg/mL, 2.0 μg/mL, 5.0 μg/mL, 10.0μg/mL and 20.0 μg/mL.
Note: The mixed standard working solution shall be stored at 0℃~4℃ for a validity period of 3 months.
4.16 Glass beads with palladium catalyst: weigh 0.04g of palladium chloride (4.6) and add 5 mL of acetic acid solution (4.13) into it; stir it slowly and heat it in a boiling bath to fully dissolve the palladium chloride, and then transfer it to an evaporating dish containing 9.5g of glass beads (4.20) (it may be washed with a small amount of water and transferred to the evaporating dish); place the evaporating dish on a water bath, heat and stir with the boiling bath to evaporate to dryness, then add water to submerge the glass beads, adjust the pH value to 8.8~9.1 with ammonia (4.1), and evaporate it to dryness again in the boiling bath; transfer the glass beads coated with palladium catalyst on the surface to a 100-mL sand core funnel, rinse the glass beads with 25mL of cyclopentane (4.5), and air-dry the glass beads for future use.
4.17 Splitless deactivated liner: matched with the injection port of the chromatograph.
4.18 Reaction liner: fill the splitless deactivated liner (4.17) with 5 mm of silanized glass wool (4.22), 2 mm of calcium carbonate (4.7), 20 mm of glass beads (4.16) with palladium catalyst, and 5 mm of silanized glass wool (4.22) in sequence from bottom to top. The filling height of the liner shall ensure that the sample injection needle does not touch the palladium catalyst layer during injection, otherwise the filling height shall be adjusted. Prior to use, the filled liner shall be aged for 1h at 300℃ at the injection port of the gas chromatograph. Determine the catalytic efficiency, r, of the reaction liner with the short chain chlorinated paraffin standard working solution (4.11), and it shall be ensured that r is greater than or equal to 80%.
4.19 pH paper: short-range pH paper, with a measuring range of 8.0~9.7.
4.20 Glass beads: with the particle size of 180μm~250μm.
4.21 Solid phase extraction cartridge: Florisil, 1g/6 mL. Prior to use, it shall be rinsed and activated with 5 mL of n-hexane (4.3).
4.22 Silanized glass wool with a maximum temperature resistance of 500℃.
Foreword i
1 Scope
2 Normative references
3 Theory
4 Reagents and materials
5 Instruments and apparatus
6 Determination procedures
7 Blank test
8 Test data processing
9 Determination lower limit, recovery rate and precision
10 Test report
Annex A (Informative) Reference chromatograms of C10, C11, C12 and C13 n-alkane standards
Annex B (Normative) Method for qualitative confirmation analysis
