GB/T 31062-2014Polymeric polyols (English PDF)

3.1 Naming of polymeric polyols

The naming of polymeric polyols consists of fixed name and feature item. The fixed name is polymer polyol, which is referred to as POP. The feature item

5.1 Determination of appearance

Load 50mLof sample into a 50mL colorimetric tube. Observe from the side.

5.2 Determination of hydroxyl value

Carry out according to the method specified in GB/T 12008.3-2009. Use Method A as the arbitration method. The sampling weighing amount is half of the amount specified in 4.5.1 of GB/T 12008.3-2009. In 4.5.2 of GB/T 12008.3-2009, after accurately weighing 25mLof phthalic anhydride acylating reagent to each test material and blank Erlenmeyer flask, add 50mL of pyridine.

5.3 Determination of water mass fraction

Carry out according to the method specified in GB/T 22313-2008.

5.4 Determination of viscosity

Carry out according to Method B specified in GB/T 12008.7-2010.

5.5 Determination of acid value

Carry out according to the method specified in GB/T 12008.5-2010.

5.6 Determination of pH value

Carry out according to the method specified in Annex B of GB/T 12008.2-2010.

5.7 Determination of solid content

5.7.1 Method summary

The non-solid components in the sample are washed by ethanol solution and separated under centrifugal force. After they are dried in a vacuum thermostat, weigh and calculate the solid content of polymer polyol.

5.7.2 Instruments and materials

This method uses the following instruments and materials:

a) High-speed centrifuge: 0r/min~16500r/min;

b) Anhydrous ethanol: analytical reagent;

c) Graduated pipette: 25mL;

d) Vacuum drying box: -0.1MPa;

5.8.2 Instruments and equipment

This method uses the following instruments and equipment:

a) Gas chromatograph: equipped with data processing device or chromatography workstation, equipped with hydrogen flame detector (FID); capillary split / split-less sample inlet;

b) Automatic headspace sample injector: 2.5mL or 1mL, graduation value is 0.001mL;

c) Headspace bottle: 20mL; equipped with silicone pad that is coated with tetrafluoroethylene on both sides and aluminum cover;

d) Analytical balance: resolution is 0.1mg;

e) Glass syringe: 1mL;

f) Polyethylene bottle: 100mL;

g) Oscillator;

h) Vacuum pump; i) Heater.

5.8.3 Test conditions

5.8.3.1 Headspace conditions

The headspace conditions of this Method are:

a) Headspace temperature: 120°C;

b) Headspace time: 20min;

c) Sample mass: 2g.

5.8.3.2 Chromatographic working conditions

The chromatographic working conditions of this method are:

a) Split / split-less sample inlet temperature: 180°C;

b) Column compartment temperature: 120°C;

c) Detector temperature: 180°C;

d) Chromatographic column: PEG20M, 0.32mm × 30m × 1µm; than 6°C.

2) Standard use solution: In 6 clean, dry 100mL polyethylene bottles, add about 100g of polymeric polyol sample without free acrylonitrile and styrene, to the nearest of 0.0001g. Respectively add 0.5g, 1g, 2g, 3g, 4g, 5g of the above standard stock solution, to the nearest of 0.0001g.

Oscillate on the oscillator for 5h. Completely mix well for use. The contents of free acrylonitrile and styrene in this standard use solution are 10mg/kg, 20mg/kg, 40mg/kg, 60mg/kg, 80mg/kg, 100mg/kg.

5.8.5 Determination steps

5.8.5.1 General

The samples taken shall be kept in sealed bottles, with little or no headspace.

The sample shall be immediately tested when it is loaded in a headspace bottle.

5.8.5.2 Preparation of curve making

In 6 pieces of 20mL headspace bottles, respectively add 2g of standard use solution. According to the test conditions of 5.8.3, conduct the headspace analysis. Record the chromatographic peak areas of acrylonitrile and styrene.

Respectively take the contents of free acrylonitrile and styrene in the standard use solution as the ordinates, the peak areas of acrylonitrile and styrene as the abscissas to draw a regression curve according to formula (2).

Where, y - Value of content of free acrylonitrile or styrene in the standard use solution, in milligrams per kilogram (mg/kg); a - Intercept of regression curve; b - Slope of regression curve; x - Peak area of acrylonitrile or styrene recorded in the standard use solution on the chromatography workstation or data processor.

5.8.5.3 Sample determination

Add about 2g of sample in a 20mL headspace bottle, to the nearest of 0.0001g.

Immediately seal. Conduct the headspace analysis according to the test conditions of 5.8.3. Record the peak areas of acrylonitrile and styrene.

5.8.6 Result calculation

The sample bottles shall be labeled to indicate the product name, specifications, batch number, sampling date and sampling staff. One bottle is for inspection and the other shall be sealed to for storage and future inspection.

6.4 Determination rules and re-inspection rules

Use the rounding-off method in GB/T 8170-2008 to round off the test results that have been inspected according to this Standard. If the inspection results meet the requirements of this Standard, it shall be accepted. If one time fails through product inspection, it shall allow re-extract the sample of double quantity from the same batch of products to reinspect the failed item. If the re-inspection results still fail, this batch of products shall be rejected.

7.1 Marks

There shall be a clear and firm mark on the packaging barrel of the product, indicating: product name, specifications, level, manufacturer name, address, production date, batch number, net mass, storage period, reference to this Standard and quality conformity mark.

7.2 Packaging

The packaging container for this product is a clean and dry paint-coated iron drum, or other pattern of clean packaging container. The lid of the packaging container must be tightly sealed with an outer lid. Each batch of products shall be attached with quality certificates.

7.3 Transport

This product can be transported by ordinary means of transportation. It shall be lightly loaded, unloaded and not upside down during transport. There shall be measures against moisture, rain, sunlight and collision.

7.4 Storage

This product shall be stored in a cool, dry and ventilated warehouse. There shall be measures to prevent sunlight and rain when storing outdoors. Under the storage and transport conditions that comply with the provisions of this Standard, the unopened products shall be stored for one year since the date of production. […]