LC-500HPLC liquid chromatography method for determination of prohibited azo dyes in textiles-Hangzhou Tianzhao Technology Co., Ltd

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LC-500HPLC liquid chromatography method for determination of prohibited azo dyes in textiles

Date: 2012-10-31Read: 0

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LC-500HPLCMethod for determination of prohibited azo dyes in textiles using liquid chromatography

1Analysis Method: GBT17592-2011 Determination of Prohibited Azo Dyes in Textiles

2 principle

Textile samples are reduced and decomposed using sodium hydrosulfite in a citrate buffer solution medium to produce potentially prohibited aromatic amines (see Appendix)A）Use appropriate liquid-Extract aromatic amines from the solution using a liquid distribution column, concentrate them, dilute with a suitable organic solvent, and use a gas chromatograph equipped with a mass selective detector（GC/MSD）Conduct measurements. If necessary, choose another or more methods to confirm the isomers. Using high-pressure liquid chromatography/Diode array detector（HPLC/DAD）Or gas chromatography/Quantitative analysis using a mass spectrometer.

3.2 Methanol.

3.3 Citrate buffer solution（0.06mol/L，pH=6.0）：取12.526gCitric acid and6.320gSodium hydroxide, dissolved in water, to a constant volume1000mL.

3.4 Sodium bisulfite aqueous solution:200mg/mLWater solution. Take solid sodium hydrosulfite before use（Na₂S₂O₄Content ≥85%）Freshly prepared.

3.5 standard solution

3.5.1 Aromatic amine standard reserve solution（1000 mg/L）

Use methanol or other suitable solvents to prepare the appendixAThe listed aromatic amine standard substances are prepared at a concentration of approximately1000mg/LReserve solution.

Note: The standard stock solution should be stored in a brown bottle and a small amount of anhydrous sodium sulfite can be placed in the freezer compartment of the refrigerator for a storage period of one month.

3.5.2 Aromatic amine standardWorking solution（20 mg/L）

Take from standard reserve solution0.2mLPlace in a volumetric flask and dilute to volume with methanol or other suitable solvent10 mL.

Note: The standard working solution can be prepared and used immediately, and other suitable concentrations can be prepared as needed.

3.6 Diatomaceous earth: Porous granular diatomaceous earth, used for600℃burn4After cooling, store in a dryer for later use.

4 Equipment and instruments

4.1 Controllable temperature ultrasonic generator: output power420W, frequency40KHzTemperature difference ±2℃；

4.2 Vacuum rotary evaporator;

4.3 Reactor: with tight closure, approximately65mLMade of hard glass in a tubular shape;

4.4 Constant temperature water bath: capable of controlling temperature（70±2）℃；

4.5 Extraction column:20cm×2.5cmGlass or polypropylene column with inner diameter, capable of controlling flow rate. When filling, first place a small amount of glass wool at the bottom, and then add it20gDiatomaceous earth（4.7）Lightly tap the extraction column to make the filling firm;

4.6 Liquid chromatograph configuration:

Pos	Product Number	Qty
1	TZ500-010	2
	High pressure infusion pump
	LC-500A Pump Includes pump, solvent cabinet, 2 solvent bottles and CAN cable.

2	TZ500-010	1
	MIXER-500static mixer
	Model 500 Mixer

3	TZ500-016	1
	Instrument Startup Kit
	HPLC Starter Kit incl. 0.17mm id cap

4	TZ500-040	1
	SPD-500Variable wavelength ultraviolet detector
	SPD-500 Variable Wavelength Detector Includes variable wavelength detector with deuterium lamp and CAN cable. No flow cell included.

5	TZ500-027	1
	7725iManual injection valve


6	TZ500-028	1
	C18 250*4.6


7	TZ500-45	1
	Solvent tray


8	TZ500-112	1
	Chromatography software
	HPLC 2D ChemStation Software For data acquisition.

9	constant temperature water bathHH-2	1
	Column temperature box


10	Sample pre-treatment package	1
	(Adjustable Temperature Ultrasonic)1Platform, vacuum pump1Table, solvent filter1Set,
	Filters and filter membranes2Package)

11	Rotary evaporator	1



12	reactor	1
	Extraction column: 20cm × 2.5cm
	Extraction device (nitrogen-containing blower)

5 Analysis steps

6.1Preparation and processing of samples

5.1.1Take representative samples and cut them into approximately5mm×5mmSmall pieces, mixed together. Weigh from the mixed sample1.0g, to0.01g, placed in the reactor（5.3）In the middle, join16mLPreheat to（70±2）℃ citrate buffer solution（4.3），Seal the reactor tightly, shake vigorously, immerse all samples in the liquid, place them in a water bath, and keep them at (70 ± 2) ℃ for 30 minutes to fully wet all fabrics.

Then, open the reactor and add3.0mLSodium hydrosulfite solution（4.4）Immediately seal and shake the reactor, then transfer it back to the reactor（70±2）Insulation in a ℃ water bath30minAfter taking it out2minCool internally to room temperature.

5.1.2Polyester products according to the appendixBThe prescribed method is used.

5.2 Extraction and concentration

5.2.1extraction

5.2.2concentrate

5.3 quantitative analysis method

5.3.1HPLCanalytical method

Due to the fact that the test results depend on the instrument used, it is not possible to provide universal parameters for chromatographic analysis. The following operating conditions have been proven to be suitable for testing.

6. Result calculation and representation

6.1 external standard method

A_i×c_i×V

X_i =……………………………………………（1）

A_iS×m

Where:

X_i—Aromatic amines are decomposed from the sampleiThe content is measured in milligrams per kilogram（mg/kg）；

A_i—Aromatic amines in the sample solutioniPeak area (or peak height);

A_is—Aromatic amines in standard working solutioniPeak area (or peak height);

c_i—Aromatic amines in standard working solutioniThe concentration is measured in milligrams per liter（mg/L）；

V—The final volume of the sample solution is measured in milliliters（mL）；

m—Sample size, in grams（g）.

6.3The results indicate

The experimental results are represented by the detection results of various aromatic amines, and the calculated results are expressed in single digits. Below the measured low *, the test result is not detected.

7 Determine the lower limit

The determination limit of this method is5 mg/kg.

8 Test Report

The test report should at least provide the following information:

a） The standards used;

b） Sample source and description;

c） The pre-treatment method used for the sample;

d） The quantitative method used;

e） Test results;

f） Any details that deviate from this standard;

g） Test date