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SN/T 5273-2020Import and export of dangerous chemicals, classification method of hazardous characteristics of tricresyl phosphate (English PDF)

进出口危险化学品 磷酸三甲苯酯危险特性分类方法

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Issued by

General Administration of Customs

Level / Type

National · Recommended

Issue date

August 27, 2020

Implementation date

March 1, 2021

Scope

SN/T 5273-2020 is the English-translated version of 进出口危险化学品 磷酸三甲苯酯危险特性分类方法.

SN/T 5273-2020 — This standard specifies the classification method for dangerous goods hazardous properties of industrial pure tricresyl phosphate. This standard applies to the classification of dangerous goods of industrial pure tricresyl phosphate.

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Document preview — SN/T 5273-2020

National Standard of the People's Republic of China

ICS
13.300
Classification
A 80

Issued by: General Administration of Customs

Contents

  • Foreword
  • Introduction
  • 1 Scope
  • 2 Normative references
  • 3 Terms and definitions
  • 4 Method summary
  • 5 Reagents and materials
  • 6 Apparatus and equipment
  • 7 Analysis steps
  • 7.1 Preparation of test solution
  • 7.2 Preparation of blank test solution
  • 7.3 Gas Chromatography-Mass Spectrometry Conditions
  • 7.4 Drawing a standard working curve
  • 7.5 Determination of samples
  • 8 Result calculation
  • 9 Judgment of hazardous characteristics
  • 9.1 Method One
  • 9.2 Method Two

Foreword

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

This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.

Drafting organization of this standard. Nanjing Customs of the People's Republic of China.

Introduction

In the United Nations "Model Regulations for Recommendations on the Transport of Dangerous Goods", tricresyl phosphate is a listed substance with a UN number 2574, the correct shipping name is "tricresyl phosphate, containing more than 3% ortho isomers", and the hazard category is 6.1.According to the United Nations the correct shipping name description of No. 2574, only when the ortho-isomer content in tricresyl phosphate is greater than 3%, the product needs to be classified as category 6.1 Toxic substances are transported, otherwise they can be classified as category 9 miscellaneous dangerous goods according to the environmental hazard data of the actual products.

United Nations No. 3082 for transportation.

In order to accurately identify the hazardous characteristics of tricresyl phosphate, a method for the determination of ortho-isomers in tricresyl phosphate was established.

Develop this standard.

Classification method for hazardous properties of import and export hazardous chemicals tricresyl phosphate

1 Scope

This standard specifies the classification method for dangerous goods hazardous properties of industrial pure tricresyl phosphate.

This standard applies to the classification of dangerous goods of industrial pure tricresyl phosphate.

2 Normative references

The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.

Recommendations on the Transport of Dangerous Goods Model Regulations (United Nations) (20th revised edition) International Maritime Transport of Dangerous Goods Regulations (United Nations) Technical Regulations for the Safety of Air Transport of Dangerous Goods (United Nations)

3 Terms and definitions

The following terms and definitions apply to this document.

Tricresyl Phosphate

Molecular formula C21H21O4P, CAS number 1330-78-5, is a colorless or light yellow transparent oily liquid, insoluble in water, soluble in Most organic solvents such as ethanol and benzene are an important chemical raw material in modern industry, mainly used as plasticizers and paint plasticizers.

The classification of hazardous properties classifies chemicals in accordance with the United Nations "Model Regulations on the Recommendation on the Transport of Dangerous Goods" (20th revised edition) (TDG), "International International regulations or national regulations such as the Maritime Transport of Dangerous Goods Regulations (IMDG), the Air Transport of Dangerous Goods Safety Technical Regulations (ICAO-TI), etc.

The industry standard conducts the appraisal of the transportation hazard to determine its transportation hazard category and degree of danger.

4 Method summary

Weigh a certain amount of tricresyl phosphate to prepare an ethyl acetate (5.1) solution, filter it through an organic filter membrane (6.2), and use gas chromatography-the mass spectrometer was used for analysis, and the external standard method was used for quantification. According to the content of tri-o-cresyl phosphate, its hazardous characteristics are determined. Phosphorus in this method the quantitative detection limit of tri-o-cresyl acid is 10 mg/kg.

5 Reagents and materials

5.1 Ethyl acetate. chromatographically pure.

5.2 Tri-o-cresyl phosphate standard product. purity >= 99%.

5.3 Tri-o-cresyl phosphate standard stock solution. accurately weigh 25 mg tri-o-cresyl phosphate standard product (5.2), accurate to 0.1 mg, Transfer to a 250 mL volumetric flask, dissolve with ethyl acetate (5.1) and dilute to the mark, and mix. The concentration of this solution is 100 mg/L.

5.4 Preparation of standard working solution. accurately pipette 0.1 mL, 0.5 mL, 1.0 mL, 2.0 mL, 4.0 mL, 6.0 mL, 8.0 mL and 10.0 mL tri-o-cresyl phosphate standard stock solution (5.3) in 8 100 mL volumetric flasks, dilute to the mark with ethyl acetate (5.1), the concentrations of the 8 standard working solutions are 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 2.0 mg/L, 4.0 mg/L, 6.0 mg/L, 8.0 mg/L and 10.0 mg/L.

6 Apparatus and equipment

6.1 Gas Chromatography-Mass Spectrometry (GC-MS).

6.2 Organic filter membrane. 0.22 µm.

6.3 Analytical balance. accurate to 0.1 mg.

7 Analysis steps

7.1 Preparation of test solution

Accurately weigh 25 mg of sample to the nearest 0.1 mg, place it in a 250 mL volumetric flask, dissolve it with ethyl acetate (5.1) and dilute to Calibrate, mix, and analyze on the machine after filtering with the organic filter membrane (6.2).

7.2 Preparation of blank test solution

Prepare a blank test solution using the reagent blank according to the method described in 7.1.

7.3 Gas Chromatography-Mass Spectrometry Conditions

7.3.1 Chromatographic column. HP-5MS 30 mm (column length) × 0.25 mm (inner diameter) × 0.25 µm (film thickness) capillary column, or equivalent.

7.3.2 Column temperature. the initial temperature is 100 °C, the temperature is increased to 220 °C at 30 °C/min, and then the temperature is increased to 300 °C at 15 °C/min, and the temperature is maintained for 5 min.

7.3.3 Temperature of the injection port. 300 °C.

7.3.4 Ion source temperature. 230 °C.

7.3.5 Carrier gas. helium (purity > 99.999%).

7.3.6 Column flow rate. 1.0 mL/min, constant flow mode.

7.3.7 Injection volume. 1 µL.

7.3.8 Sampling mode. splitless sampling.

7.3.9 Solvent delay time. 5 min.

7.3.10 Transmission line temperature. 280 °C.

7.3.11 Mass spectrum scanning mode. Selected ion monitoring (SIM) mode.

7.3.12 Qualitative ion and quantitative ion. see Table 1.

7.4 Drawing a standard working curve

According to the determination conditions listed in 7.3, the standard working solution (5.4) is injected for determination in the order of concentration from low to high. By standard the concentration of tri-o-cresyl phosphate standard (5.2) in the solution is the abscissa, and the unit is milligrams per liter (mg/L).

The chromatographic peak area of cresyl ester is the ordinate, and the standard curve is drawn. Refer to Appendix A for a typical gas chromatography-mass spectrogram of tri-o-cresyl phosphate.

ys--The chromatographic peak area of tri-o-cresyl phosphate;

a --The slope of the regression curve;

xs--The concentration of tri-o-cresyl phosphate in the standard working solution, in milligrams per liter (mg/L);

b - The intercept of the regression curve.

7.5 Determination of samples

The sample test solution (7.1) and blank test solution (7.2) are also injected and analyzed according to the gas chromatography-mass spectrometry conditions listed in 7.3.

In addition to the blank value, the chromatographic peak area of tri-o-cresyl phosphate in the sample is obtained.

When the concentration of the tri-o-cresyl phosphate standard product (5.2) in the sample test solution (7.1) is greater than the upper limit of the concentration of the standard curve, the the test solution is appropriately diluted with ethyl acetate (5.1) to ensure the content of tri-o-cresyl phosphate standard product (5.2) in the diluted test solution Within the concentration range of the standard curve.

8 Result calculation

The content of tricresyl phosphate in tricresyl phosphate is calculated according to formula (2).

X-the content of tri-ortho-cresyl phosphate in tricresyl phosphate, in milligrams per kilogram (mg/kg);

y-the chromatographic peak area of tri-o-cresyl phosphate in the sample test solution;

b-the intercept of the regression curve;

250 --- the constant volume of the test solution, the unit is milliliters (mL);

n - the dilution factor of the test solution;

a --The slope of the regression curve;

m-Weigh the sample size, the unit is grams (g).

9 Judgment of hazardous characteristics

9.1 Method One

According to the overall health toxicity and ecotoxicity data of tricresyl phosphate, compared with the UN Recommendations on the Transport of Dangerous Goods the hazard classification standards in Section 2.6.2.2 and Section 2.9.3.3 of the Model Regulations determine the hazard category and packaging level of the product.

9.2 Method Two

If the content of tricresyl phosphate in tricresyl phosphate is more than 30 000 mg/kg (ie 3%), the According to the classification standard established by the Recommended Model Regulations for the Transport of Goods, the product should be transported according to UN No. 2574, and the hazard category it is a category 6.1 toxic substance.

If the content of tricresyl phosphate in tricresyl phosphate is less than or equal to 30 000 mg/kg (ie 3%), the According to the classification standards determined by the Recommendations for the Transport of Dangerous Goods, the product should be transported in accordance with UN No. 3082.

Not classified as category 9 miscellaneous substances and articles.

Appendix A

(Informative appendix) Typical gas chromatography-mass spectra of tri-o-cresyl phosphate

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

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