ICS 75.

140 STAS 8099-74

A 57

ROMANIAN STANDARDS

BITUMENS
Determination for loss of mass by heating

Official Edition
STAS 8099-74 -2-

Drawn up by: Ministry of Chemical Industry

Institute of Research and Design of the Ploiesti Refinery
Project manager: Eng. Grigore Stejaru

Partners: Industrial Plant of Refineries and Petrochemistry – Ploiesti

Institute of Studies and Research for Transport – Bucharest
Institute of Research and Design for Industry of Construction Materials – Bucharest
Teleajen Refinery
Station for Conditioning, Delivery and Transport of Mineral Oil – Bucharest
Ploiesti Refinery
Trust for Isolations for Industrial Works – Bucharest
Ploiesti Nord Refinery

Final editing: ROMANIAN STANDARDS INSTITUTE

Department of Mines, Oil, Chemistry
Eng. Doina Sandu

Certified by: Standard Committee for Mines, Oil, Chemistry

Approved by: ROMANIAN STANDARDS INSTITUTE

Date of approval: July 27th, 1973

Nota Notice
Metoda II corespunde cu RS CAER 2971-71. The 2nd method is in accordance with CMEA
Standardul a fost elaborat iniţial in 1968 şi revizuit RS 2971-71.
în 1973. The standard was initially drawn up in 1968 and
revised in 1973.

ASOCIAŢIA DE STANDARDIZARE DIN ROMÂNIA (ASRO),

Adresa poştală: str. Mendeleev 21-25, 70168, Bucureşti 1, Direcţia Generală: Tel.: +40 1 211.32.96; Fax: +40 1 210.08.33,
Direcţia Standardizare: Tel. : +40 1 310.43.08; +40 1 310.43.09, Fax: +40 1 315.58.70,
Direcţia Publicaţii: Serv. Vânzări/Abonamente: Tel: +40 1 212.77.25, +40 1 212.79.20, +40 1 212.77.23, +40 1 312.94.88 ;
Fax : +40 1 210.25.14, +40 1 212.76.20
 ICS 75.140

ROMANIAN STANDARD STAS 8099-74

Classification index A 57
Replacing:
BITUMENS STAS 8099-68
Determination for loss of mass by heating Previous editions:

Bitumuri - Determinarea pierderii de masă prin încălzire

Validation date:
Bitumes - Détermination des pertes de masse par chauffage 1974-02-01

1 GENERAL

1.1 This standard refers to the determination for the loss of mass by heating of bitumens.

1.2 The loss in weight is determined by two methods:

st
– 1 method
– 2nd method
The method used is mentioned in the product standard.

1.3 The methods are also used for the determination of the stability of bitumens at high temperatures,
pointed out by the modification of values of some characteristics of the bitumen specimen under investigation such as
softening point, penetration at 25 0 C and Frass breaking point.

2 FIRST METHOD

2.1 Principle of the method

The method consists of the determination for loss of mass of the bitumen after it has been heated for 5 hours at
163 0C in an oven.

2.2 Equipment

─ Flat bottom cylindrical brass flask, 55 ± 1 mm in diameter and 35 ± 1 mm in height.

─ Heat controlled oven which can maintain the temperature with an accuracy of ± 10 C.
─ Graduated thermometer comprising the interval of temperatures between 155 ….. 170 0 C, with the value of
division of 0.5 0C.

2.3 Determination preparation

2.3.1 The bitumen specimen is dehydrated by heating and continuous mixing at a temperature with
80 … 100 0C higher than its softening temperature, without exceeding the value of 200 0 C.

2.3.2 The still fluid dehydrated bitumen is filtered through a gauze-wire screen 071 STAS 1077-67 and
mixed with a rod till the bubbles escape.

ASOCIAŢIA DE STANDARDIZARE DIN ROMÂNIA (ASRO),

Adresa poştală: str. Mendeleev 21-25, 70168, Bucureşti 1, Direcţia Generală: Tel.: +40 1 211.32.96; Fax: +40 1 210.08.33,
Direcţia Standardizare: Tel. : +40 1 310.43.08; +40 1 310.43.09, Fax: +40 1 315.58.70,
Direcţia Publicaţii: Serv. Vânzări/Abonamente: Tel: +40 1 212.77.25, +40 1 212.79.20, +40 1 212.77.23, +40 1 312.94.88 ;
Fax : +40 1 210.25.14, +40 1 212.76.20

© ASRO Entire or partial multiplication or use of this standard in any kind of publications and by any means (electronically, mechanically,
photocopy, micromedia etc.) is strictly forbidden without a prior written consent of ASRO
STAS 8099-74 -2-

2.4 Working procedure

2.4.1 For one determination 2 clean and dry brass flasks are separately weighed with an accuracy of 0.01 g,
to constant weight.
2.4.2 After cooling, the still fluid bitumen is casted in the flasks in a thick layer of approximately 25 mm. It
is left to cool to ambient temperature keeping the dust off, then the flasks containing bitumen are weighed with an
accuracy of 0.01 g.

2.4.3 They are introduced in an oven heated at 163 ± 10 C and maintained at the same temperature for
5 hours.
NOTE – Because the temperature drops after the introduction of the flasks in the oven, the 5 hour time is considered only
after the temperature returns at 163 ± 1 0 C. The time in which the temperature comes back to 163 ± 1 °C shall not exceed
15 minutes.

2.4.3 After 5 hours the flasks containing bitumen are taken out of the oven, introduced in a desiccator for
cooling till they reach ambient temperature then weighed separately with an accuracy of 0.01 g.

NOTE – No more than 2 flasks with bitumen shall be heated in the oven at the same time.
It is not permitted to heat more than 2 flasks with bitumen in the same time.

2.5 Calculation

Loss in weight is expressed as a percentage with two decimals and is calculated from the formula:

m−m1
% Loss of mass = 100
m
where:
m is the mass of bitumen before heating, in g.
m1 is the mass of bitumen after heating, in g.

The result of the determination is the arithmetical average of the two obtained values, which shall not differ
with more than 0.03 % in absolute value.

2.6 Admitted differences

The result is the arithmetical average of two determinations the results of which shall not differ with more than
the values from table 1.

Table 1
Admitted differences
Loss of mass,
% Repeatability, Reproducibility,
% %
Below 0.5 0.05 in absolute value 0.10 in absolute value
Over 0.5 up to 1.0 0.10 in absolute value 0.20 in absolute value
Over 1.0 up to 2.0 0.15 in absolute value 0.30 in absolute value
Over 2.0 5 of the average 10 of the average

3 SECOND METHOD

3.1 Principle of the method

The method consists in the determination of loss in weight of the bitumen after a heating for 5 hours at 1630 C.

3.2 Equipment

─ Cylindrical brass flasks with the following sizes:

─ diameter ……………………………………… 128 ± 1 mm
 -3- STAS 8099-74

─ height ………………………………………… 15 ± 0.5 mm

─ wall thickness ………………………………… 1.5 ± 0.1 mm
─ Heat controlled oven which can maintain the temperature with an accuracy of ± 1 0C with a capacity of
minimum 20 l. The diameter of the superior air opening shall be 15 to 20 mm. The oven shall have a perforated metallic
disk, with a diameter of approximately 25 cm, placed at the center of the oven suspended by a vertical axe.
The disk rotates with a speed of 5 … 6 r/min.
─ Graduated thermometer which can comprise the interval of temperatures between 155 ….. 170 0C, with the
value of division of 0.5 0C.
─ Gauze-wire screen 071 in accordance with STAS 1077-67.

3.3 Determination preparation

3.3.1 The bitumen specimen is dehydrated by heating and continuous mixing at a temperature 80 … 100 0C
higher than its softening temperature, without exceeding the value of 200 0C.

3.3.2 The still fluid dehydrated bitumen is filtered through a gauze-wire screen 071 STAS 1077-67 and
mixed with a rod till the bubbles escape.

3.4 Working Procedure

3.4.1 The clean and dry brass flasks are separately weighed with an accuracy of 0.01 g, to constant mass.

3.4.2 For one determination, there are casted in each of the 3 flasks 50 ± 0.1 g of the bitumen prepared in
accordance with clause 3.3. The bitumen is levelled in an uniform layer by inclining the flasks in all directions.

3.4.3 After cooling the bitumen to ambient temperature, the flasks containing the specimens are weighed
with an accuracy of 0.01 g.

3.4.4 The weighed flasks are placed on a an asbestos plate on the disk in the oven, at a temperature of 163 ±
10 C and the disk is rotated during the whole determination with a speed of 5 … 6 r/min.

3.4.5 The temperature is determined using the thermometer fixed on the axe of the disk in vertical position,
at approximately 2 cm from the center of the axe and above the layer of bitumen in the flasks.

3.4.6 The flasks are taken out of the oven after 5 hours, cooled in a desiccator, to ambient temperature and
weighed with an accuracy of 0.01 g.

3.5 Calculation

The loss of mass is expressed as a percentage with two decimals and is calculated with the formula:

m − m1
% Loss of mass = 100
m
where:
m is the mass of bitumen before heating, in g.
m1 is the mass of bitumen after heating, in g.

The result of one determination is the arithmetical average of the two values obtained, which shall not differ
with more than 0.2 % in absolute value.
STAS 8099-74 -4-

3.6 Admitted differences

The result is given by the arithmetical average of two determinations, the results of which shall not differ with
more than the values from table 2.

Table 2
Loss of mass, Admitted differences, % in absolute value
% Repeatability Reproducibility,
Below 0.2 0.05 0.08
From 0.2 to 1.0 0.10 0.15
Over 1.0 0.15 0.25

4 DETERMINATION OF THE BITUMEN CHARACTERISTICS MODIFICATION

AFTER HEATING

In case there is also required a determination of the modification of values of bitumen characteristics after
heating, the procedure is as follows:

The content of the flasks remained after the determination of loss in mass is melted, by introducing them in an
oven at a temperature of approximately 1600 C (maximum 15 minutes), mixing and then there are determined, if
required, for the following characteristics:
─ softening point in accordance with STAS 60-69;
─ penetration at 250 C in accordance with STAS 42-69;
─ Fraass breaking point in accordance with STAS 113-74.

5 INPUTS IN THE TEST REPORT SHEET

The test report sheet comprises the following elements:
─ data necessary to identify the product,
─ method used,
─ results obtained,
─ STAS 8099-74.