Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by China National Textile and Apparel Council.
This standard is under the jurisdiction of the Basic Standard Subcommittee of the National Technical Committee on Textiles of the Standardization Administration of China (SAC/TC 209/SC 1).
Textiles - Determination of fluorescent brighteners
Warning – Persons using this standard shall be familiar with normal laboratory practice. 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 measures and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the method for determining nine fluorescent brighteners in textiles (see Annex A) with high-performance liquid chromatograph - fluorescence detector (HPLC-FLD).
This standard is applicable to various textiles.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated reference, only the edition cited applies. For undated references, the latest edition of the referenced documents (including any amendments) applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principle
The specimen is placed in the mixed solution of dimethyl formamide and water. After ultrasonic extraction, it is determined by high-performance liquid chromatograph equipped with fluorescence detector (HPLC-FLD). The retention time is used for qualitative analysis of the to-be-determined substance, and the external standard method is used for quantitative analysis of the to-be-determined substance.
4 Reagents and materials
4.1 Unless otherwise specified, water for analysis shall be Grade III water specified in GB/T 6682.
4.2 Methanol: chromatographically pure.
4.3 Acetonitrile: chromatographically pure.
4.4 Trichloromethane: chromatographically pure.
4.5 Dimethyl formamide: analytically pure.
4.6 Ammonium acetate: chromatographically pure.
4.7 Mixed solution of 70% dimethyl formamide and water (volume ratio): take 700ml of dimethyl formamide, add water to 1,000ml and mix well for later use.
4.8 20mmol ammonium acetate solution: take 1.54g of ammonium acetate (4.6), add Grade I water (specified in GB/T 6682) to dissolve it to 1,000ml, and mix well for later use.
4.9 Standard substance: fluorescent brightener standards, see Annex A.
4.10 Standard stock solution:
Accurately weigh about 50.0mg (to the nearest of 0.000 1g) of standard substances (4.9) of fluorescent brighteners C.I.85, C.I.113, C.I.351 and C.I.71 and put them into 50mL volumetric flasks respectively, dissolve them with mixed solution of 70% dimethyl formamide and water (4.7) and dilute to the scale (for fluorescent brightener 71, a small amount of mixed solution of 70% dimethyl formamide and water shall be added for ultrasonic dissolution, and then dilute to the scale) in order to prepare the standard stock solution with a mass concentration of 1mg/mL.
Accurately weigh about 50.0mg (to the nearest of 0.000 1g) of standard substances (4.9) of fluorescent brighteners C.I.162, C.I.140, C.I.135, C.I.199 and C.I.220 and put them into 50ml volumetric flask respectively, then add trichloromethane to prepare standard stock solution with mass concentration of 1mg/mL.
Note: The above standard stock solution shall be stored in a refrigerator under cold storage conditions, and it has been proved to be feasible to store the solutions within 6 months; as trichloromethane is a highly toxic substance, operators shall pay attention to personal safety.
4.11 Mixed standard working solution (original):
Accurately pipette an appropriate amount of standard stock solution (4.10) (see Table 1) and transfer it into a 100mL volumetric flask, then dilute the solution with acetonitrile to the scale to prepare mixed standard solution (original) of fluorescent brightener. See Table 1 for the concentration.
Table 1 Preparation instruction of mixed standard working solution (original)
No. Name Pipetted volume of standard stock solution / mL Constant volume solution Constant volume / mL Concentration after dilution / (μg/mL)
1 Fluorescent brighteners C.I.220 7 Acetonitrile 100 70
2 Fluorescent brighteners C.I.85 4 40
3 Fluorescent brighteners C.I.113 4 40
4 Fluorescent brighteners C.I.351 0.1 1
5 Fluorescent brighteners C.I.71 2 20
6 Fluorescent brighteners C.I.162 1 10
7 Fluorescent brighteners C.I.140 0.4 4
8 Fluorescent brighteners C.I.135 0.1 1
9 Fluorescent brighteners C.I.199 0.2 2
Note: The above mixed standard working solution (original) of fluorescent brightener shall be stored in a refrigerator under cold storage conditions, and it has been proved to be feasible to store the solution within three months.
5 Apparatuses
5.1 High-performance liquid chromatograph: equipped with fluorescence detector.
5.2 Ultrasonic cleaner: with ultrasonic power no less than 270W, ultrasonic frequency of 50/60kHz, and the temperature control range from 25℃ ~ 80℃.
5.3 Balance: with divisions of 0.0001g and 0.01g.
5.4 High speed centrifuge: with available rotational speed of 5,000r/min.
5.5 Organic filter membrane: with a pore diameter of 0.45μm.
5.6 Glass reaction flask with stopper: 50mL.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Apparatuses
6 Analytical procedures
7 Result calculation
8 Low determination limit, recovery rate and precision
9 Test report
Annex A (Normative) Basic information of nine fluorescent brighteners
Annex B (Informative) Relevant detection information of nine fluorescent brighteners
Annex C (Informative) Liquid chromatograms of nine fluorescent brighteners in textiles
