SN/T 0152-2014Method for inspection of 2, 4-D residues in fruit for export (English PDF)

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules.

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This standard replaces SN 0152-1992 "fruit for export 2,4-D residues in." this standard compared with SN 0152-1992, the main changes are as follows.

--- Text structurally different. SN 0152-1992 according to GB/T 1.1-1987 prepared, according to the present standard GB/T 1.1-2009 and GB/T 20001.4-2001 write;

--- Expanding the scope of the detection object;

--- Delete the sample content (see the 1992 version of Chapter 2);

--- Increasing the sample stored content (see Chapter 6);

--- Reagent derived from "n-butanol and boron trifluoride solution" to "n-butanol and concentrated sulfuric acid";

--- Florisil - alumina column into florisil solid phase extraction columns for sample clean-up;

--- Increasing the lower limit of determination and recovery (see Chapter 8).

This standard is proposed and managed by the National Certification and Accreditation Administration Committee.

This standard was drafted. People's Republic of China Hunan Exit Inspection and Quarantine.

1 Scope

This standard specifies the gas chromatographic determination of apples, pears, bananas, pineapple and citrus 2,4 pesticide residues.

This standard applies to the determination of pesticide residues in 2,4 apples, pears, bananas, pineapple and citrus.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.

Laboratory use specifications and test methods GB/T 6682 Analysis

3 Method summary

Samples with phosphoric acid - acetone solvent extraction, liquid - partition purification, concentrated sulfuric acid as a catalyst, with n-butanol 2,4 2,4 esterified Butylate, and then Florisil SPE column purification, determined by gas chromatography, external standard.

4 Reagents and materials

Unless otherwise specified, reagents were of analytical grade, test water should be consistent with GB/T 6682 three water indicators.

4.1 acetone. HPLC grade.

4.2 phosphoric acid. 85%.

4.3 chloroform.

4.4 ether.

4.5 hydrochloric acid. 36% to 38%.

4.6 Concentrated sulfuric acid. pure class, 95% to 98%.

4.7 n-butanol.

4.8 hexane. HPLC grade.

4.9 sodium hydroxide.

4.10 disodium hydrogenphosphate.

4.11 anhydrous sodium. 650 °C burning after 4h, stored in a desiccator.

4.12 phosphoric acid (11).

4.13 aqueous hydrochloric acid (11).

4.14 phosphate solution. Weigh 2g of sodium hydroxide (4.9) and 44g of disodium hydrogen phosphate (4.10), dissolved in water and diluted to 1000mL.

4.15 sodium sulfate solution (20g/L). Weigh 2g of anhydrous sodium sulfate (4.11) were dissolved in 100mL water.

4.16 acetone - n-hexane (19).

4.17 2,4-D standards. purity not less than 99.0%, CAS Number. 94-75-7.

4.18 2,4-standard stock solution. Weigh accurately 0.01000g2,4- drop standard (4.17) in 10mL flask with about 8mL prop One was dissolved with acetone to volume, standard stock solution to give a concentration of 1.0mg/mL, and stored at 4 °C refrigerator.