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GB/T 35930-2018Determination of vapor pressure of chemical products—Thermogravimetry method (English PDF)

化工产品饱和蒸气压的测定 热重法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

February 6, 2018

Implementation date

September 1, 2018

Scope

GB/T 35930-2018 is the English-translated version of 化工产品饱和蒸气压的测定 热重法.

GB/T 35930-2018 describes how to determine the vapour pressure of solid and liquid chemical products by thermogravimetry.

The sample is held at a series of isothermal steps under a slow inert gas flow and its rate of mass loss is recorded; the linear relationship between the logarithm of vapour pressure and that rate gives the saturated vapour pressure at each temperature, and values at 20 °C and 25 °C can be extrapolated from the regression of ln p against 1/T. The standard specifies the thermobalance, with a furnace reaching 450 °C and a balance sensitivity of ± 10 µg, benzoic acid as reference substance and dried nitrogen as carrier gas.

It also covers the procedure, results and test report, with benzoic acid vapour pressure data in Annex A. It was issued on 6 February 2018 and has applied since 1 September 2018.

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Document preview — GB/T 35930-2018

National Standard of the People's Republic of China

ICS
71.040.01
Classification
G 04

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope4
  • 2 Principle for test method4
  • 3 Apparatus4
  • 4 Reagents and materials5
  • 5 Analytical procedures5
  • 6 Result analysis and treatment6
  • 7 Test report7
  • Annex A (Informative) Vapor pressure data of benzoic acid8

1 Scope

This Standard specifies the method for the determination of vapor pressure of chemical products using the thermogravimetry method.

This Standard applies to all solids and liquids of saturated vapor pressure within the range of 1-10 Pa ~ 1 Pa.

Impurities in chemical products have a certain influence on vapor pressure results during measurement.

2 Principle for test method

In this Standard, thermogravimetric analysis meter is used to determine the speed of loss in mass within a certain time under relatively high temperature and indoor pressure. Under a slow inert gas flow atmosphere and temperature T (in K), the loss in mass of sample is monitored within a certain time to obtain the speed of loss in mass vT. Based on the linear relationships between vapor pressure logarithm and the speed of loss in mass, saturated vapor pressure pT at temperature T can be calculated from vT. If necessary, vapor pressure under 20°C and 25°C can be extrapolated from the regression between 1npT and 1/T.

3 Apparatus

3.1 Thermogravimetry analysis meter, which is equipped with the following devices.

3.1.1 Thermo-balance, including the following elements.

a) furnace chamber. capable of staying at a constant temperature and heating sample to 450°C at a constant speed of 5°C/min ~ 25°C/min;

b) temperature sensor. used to display the temperature of sample/furnace chamber, with a sensitivity of ± 0.1°C;

c) continuous record balance. with a sensitivity of ± 10 µg;

d) controlled inert gas atmosphere device. with a purity of inert carrier gas above 99.99% and rate of flow (0 mL/min ± 5 mL/min) ~ (100 mL/min ± 5 mL/min).

3.1.2 Temperature controller. capable of executing specific temperature programs within temperature intervals selected, with a temperature change ratio of 0°C/min ~ 25°C/min and temperature fluctuation within ± 0.5°C.

3.1.3 Recording unit. capable of recording and displaying the mass signals of sample and the changes of noise signals to temperature and noise (the TGA Curve).

3.1.4 Crucibles. their area can be measured; they will not react with sample; they can remain stable under 450°C.

3.2 Graduated micropipettes. with a capacity of 20 µL ~ 40 µL and tolerance ± 1 µL.

4 Reagents and materials

4.1 Benzoic acid. with a purity not lower than 99.9%.

4.2 Nitrogen. with a purity of 99.99% (or other inert carrier gases). It is dried using molecular sieve or silica gel.

5 Analytical procedures

5.1 Sample pre-treatment

Apply liquid sample evenly on the surface of crucible (3.1.4). If sample is a solid, semi-solid or viscous liquid, it can be dissolved using an appropriate solvent and then infiltrated on the surface of crucible (3.1.4) using a solution.

5.2 Sample determination

5.2.1 Place crucible (3.1.4) applied with sample in the test chamber of thermogravimetric analysis meter; dry to a constant weight in a nitrogen (4.2) atmosphere. Adjust nitrogen (4.2) flow which shall not be too high, to ensure that gasified molecules can be taken away in time.

5.2.2 Set the temperature control procedure which consists of a series of isothermal sections. Maintain a temperature difference of 10 K between temperature sections. If another temperature is used, it shall be indicated in report. Maintain for a certain time before starting each temperature section; set 10 min or longer time of constant temperature. The increase of constant-temperature time is normally to be benefit of stable volatilization, but it will extend test time.

5.2.3 The lower limit of constant-temperature range is subjected to that there needs to […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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