☠ Safety warning: The reagents used in the test method, such as phenol and tetrachloroethane, are toxic.

Be sure to take safety precautions to

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avoid skin contact and inhalation of its vapor, and operate in a fume hood as much as possible.

Reference Standard：
GB／T 1632.5-08 (Capillary viscometer for plastics to measure the viscosity of dilute polymer solutions)
GB／T 14190—2017 (Fiber-grade polyester chip analysis method)
ISO 3105 (Glass capillary kinematic viscometer specifications and operating instructions)
ISO 1628—5：1998 (Thermoplastic polyester homopolymers and copolymers Polybutylene terephthalate (PBT)-polyester Polyethylene
terephthalate (PET)-polyester resin)
ASTM D 4603 (Standard Test Method For Determining Inherent Viscosity Of Poly(Ethylene Terephthalate) (PET) By Glass
Capillary Viscometer)

Method summary
Measure the time for the solvent at 25°C and the PET solution with a concentration of 0.005g/mL to flow out of the capillary, and calculate the
intrinsic viscosity based on the measured flow time and the solution concentration of the sample to meet the requirements that the kinetic energy
calibration item of the viscometer is not considered.
1.1 Instruments and Equipment

No. Instrument Name Accuracy/ Specifications Application

1 IVS400 Automatic Viscometer ±0.01 Viscosity Test
2 Polymer sample dissolver P12 ±1℃ Dissolving
3 Analytical Balance 0.1mg Weighing
4 Automatic pipette or manual pipette 25ml Pipetting
5 Glass Sand core funnel G2 Filtering
6 High precision thermometer 0.01 Temp Calibrate
7 Ubbelohde Viscometer Tube Testing
8 Heater & Stirrer Making Solvent

1.2 Reagent

No. Reagent Name Ratio

1
Phenol（AR）
2 1,1,2,2-Tetrachloroethane(AR)
3 Phenol/1,1,2,2-Tetrachloroethane (Mass Ratio 60:40) Weight VS Weight
4 Concentrated sulfuric acid
5 Deionized water or pure water
6 Anhydrous ethanol
Precautions：
1. Organic solvents are harmful to the human body, wear natural rubber gloves and gas masks
2. Phenol is crystalline at room temperature (melting point: 43°C), completely dissolved at 55-65°C in advance (drying oven or water bath)
for 6 hours. You can take out the bottle and shake to check if it is fully dissolved.
Please note, the smell is bad while using drying oven. It is suggested to use water bath.
3. It is suggested to prepare the solvent in 1 L or 2L ,as it can be used for 30 days. And no need to prepare the solvent / test solvent viscosity
every day.
4. Solvent prepare.
a) When phenol dissolved finished, the phenol is hot.
b) Take 1L brown bottle to place on the balance, set weight 0.
c) Fill the hot phenol to the bottle, and get the weight, such as 600.00g.
d) Set the balance weight 0.
e) Fill the 1,1,2,2 Tetrachloroethane to the bottle, make the weight is 400.00g.
5. When solvent prepared, place them in a constant temperature source at 25°C and stir for 24 hours.
Check their density with a hydrometer, adjust to the required range, (3:2 ,25±0.02℃ Density 1.235±0.003g/cm3)
4. The configured solution cannot be used for more than one month. The solvent should be stored in a brown glass bottle, protected from light,
and placed at an ambient temperature of 25°C to avoid crystallization. So, best way is to place the bottle on a stirring machine with heating
temp 25°C all the time.
When ever need, take out 50ml or 25ml for test.
When solvent/ tube/measure unit not changed, solvent IV no need to test every time.
2. Experiment Procedure

2.1 Preparation before experiment

No. Operation Procedure Specific Description Photo

1 The raw material inspector obtains the sample to be tested in accordance with the
Sampling
<Regulations on Sampling of Raw and Auxiliary Materials>

1. Place the constant temperature water bath and chiller on a firm and stable horizontal
working desk and connect the water pipe to add pure water (best suggested deionized water,
or Ethylene Glycol and deionized water 1:1).
2. Put the measuring unit into the water bath and connect the gas line, liquid pipe and electric
line. (See the installation diagram for details).
3. Turn on the thermostatic water bath and chiller.
4. Set the target temperature and stable at 25±0.01°C (or 30 ±0.01°C).
5. After the equipment is working normally, check before the daily experiment: the liquid
2 Instrument level of the waste liquid bottle, The vacuum pump, the water level alarm light of the water
Preparation bath, and the indicator light of the measuring table.
Precautions：
1. The water level is a slightly different indicator bin for the measurement chamber. If the
water level alarm is on, please check whether the water level is normal. Judgment criteria:
the inner circulating water flows from the bin to the supervision chamber, and the outer
circulating water flows from the mixing bath to the chiller, and the outer liquid The best
side difference is 3-5cm.
2. The liquid level of the waste liquid bottle should be drained by 3cm. If it exceeds, the waste
No. Operation Procedure Specific Description Photo
liquid bottle should be emptied in time before the test.
3. The working indicator of the measuring table is not on, please turn off the main controller
in time and check the circuit.
No. Operation Procedure Specific Description Photo
1. Accurately weigh 0.1250±0.0002g sample into the sample dissolving bottle, add 25ml
blank solvent that has been stirred for 24h. according to the standard, the concentration is
0.005 g/ml
2. Place in the sample dissolver, stir and heat for 25min, take it out and cool to room
temperature
Dissolution temperature: fiber-grade standard chips , 95℃;
Bottle grade polyester chips, 110℃
Speed: 450 rpm
3 Sample Processing
Precautions:
1. If the moisture content of the sample is greater than 0.5%, put the chips in a vacuum drying
oven at 133.3Pa, 105°C, dry for 3 hours, and put them in a desiccator to cool.
2. Moisture has a great influence on the experiment and will cause large errors. Be careful not
bring moisture during the experiment.
3. Dissolve the sample according to the specified temperature and time to prevent over-
temperature degradation or uneven sample dissolution. Carefully check whether the
dissolution is complete (take out bottle and watch )and beware of polymer particles sticking
to the bottle wall and not dissolving into the dissolving bottle.
1. Put the viscometer tube into the holder and place it on the measuring unit.
2. Install the glass sand core funnel for manual filtering of samples, cleaning agents, etc.
3. Install the discharge pipe and extend the elbow to the elbow of the viscometer tube.
4 Tubes Preparation
Precautions:
1. Check whether the viscometer tube diameter is appropriate and whether the sand core
funnel model is appropriate.
No. Operation Procedure Specific Description Photo
2. Put the tube into the measuring unit vertically, and lightly press the pressure block to seal
it.

2.2 Software Parameter Setting

No Operation Content and Pictures

. Steps
1. Click "Method" in the menu interface, click "Setting New " in the "Method" interface, and the following interface will
appear.
1 Method 2. In "Create Method", set the unit number.
Setting 3. In the "test method", fill in the name of the test method, such as: blank viscosity, sample viscosity, cleaning agent.
4. Change the options in the "standard method", different test items will appear, which can be selected according to the test
method, such as: solvent viscosity, Billmeyer, lift cleaning, etc.
5. The Data of "Absolute deviation" should be set according to specific industry standards, and its type is based on the
content selected in the menu bar -> System Management -> Settings -> Deviation Type.
"Viscometer tube number" line: It can be filled in according to the actual parameters, or press to load the parameters
from the saved tube list.
Other data will be loaded into the data of the previous operation, should be modified according to the actual situation,
and will appear as an index item in the saved historical data.
6. In the same way as above, each unit establishes "blank viscosity", "sample viscosity", "cleaning agent ", "cleaning agent
drying" and other methods. After the test method is established, save them. If not applicable, you can edit them. Delete
and other operations.
7. The picture is an example of PET, the parameters are just for reference, and the specific description of the parameters
can be found in the software settings.
No Operation Content and Pictures
. Steps
Method one:
1. Click "Task" in the menu interface, the window shown in the figure below, click the + sign, you can see the various
methods set in "Methods", select tasks according to the test sequence.
2. Under each unit, set options such as "rinse", "out of tolerance retest", "draining", etc., and tick them as needed.
Rinse: it means, when fille the sample ,the machine will run the wash and discharge program. That is why we use half
of the sample fill in to tube, and rinse, Half for the test.
Out of tolerance retest: When we set the solvent test , absolute deviation 0.1 s, sample test absolute deviation 0.2s.
The max value- min value is over 0.1s or 0.2s, the machine will add extra test.
2 Task
configuratio
n

Draining: it means, when test finish, the result is true, the machine will discharge the solvent or simple automatically.Then
waiting you to fill the wash agent and wash the tubes.
Method 2
1. Click "Main Interface" in the menu, click "Select Method", select the testing method "Blank Viscosity", "Sample
Viscosity", "Cleaning Agent Cleaning" or "Cleaning Agent Drying", and set the parameters in each method. You can
refer to the software parameter description.
2.3 Viscosity Measurement Process

No. Operation Steps Specific Description

1. It can be used after the temperature of the water bath stabilizes at 25±0.01℃. (Verify with a 0.01℃ high-
precision thermometer)
2. Detect the viscosity of the blank solvent
1) Before all samples on the test, only need to test one set of blank solvent outflow time. If two test units
are used, two blanks needed tested; if one test unit is used, one blank is tested.
2) The number of times of each blank test is (1+3).
3) Set the blank solvent Absolute deviation value 0.1s(or standard deviation 1%), The data exceeds 0.1s (or
1%), the solvent needs to be reconfigured, and the detection method choose blank)
1 Viscosity Test
3. Detect multiple samples such as the sample to be tested 1, 2, 3, etc. ( Choose the detection method as
sample).
4. Data Processing
Precautions：
1. Cleanliness of the tested solution: the solvent and solution entering the viscometer tube should be
filtered with a stainless steel filter of 600 mesh or more or a G2 glass sand funnel. Solvents and
solutions should not use the same filter, otherwise they must be thoroughly cleaned and dried.
1. Use a blank solvent for the first-time cleaning (choose cleaning A for the cleaning method)
2. Use absolute ethanol for the second time cleaning and drying (the cleaning method is cleaning B)
2 Cleaning
Reagent bottle cleaning: Recycle the waste liquid in the reagent bottle to the waste liquid collection bottle, put
the glass sand core and bottle in lye (1%) soaked for no less than 2h, then take it out, then put in detergent and
wash it with a brush, and finally After cleaning with water, put it in an oven to dry for later use.
No. Operation Steps Specific Description
1. Data sorting: Find the test data of the day in the "historical data", save it, sort it out, and then register.
2. Instrument shutdown: After the test task is over, turn off the instrument. First turn off the chiller, then turn
3 Sorting
off the host; if you need to run for a long time, pay attention to observe the liquid level in the bath, and the
indicator on the MARK meter, which is below the warning interface, please add water in time.
Explain of Rinse, Out of tolerance retest, Draining.

Rinse: When click this, when the test start.

1. The software will remind you to use half of the sample volume in the tube.
2. When filled, click confirm.
3. Machine will wash the tubes automatic and discharge the waste liquid.
4. Software reminds you to fill the rest of the sample and start the test.
Out of the tolerance retest.

For example, the result over 0.2s, the machine will add extra test(flow time D).
If extra test still over 0.2s, the machine will restart the test 3 time.

² If the “Out of the tolerance retest” not been chosen.

² When first test finished, deviation over 0.2s, machine will add extra test (flow time D), and flow time D still over 0.2s, the machine will fails
and stop waiting for operator.

Draining: When test finished, the result is true. The machine will discharge the testing sample automatic.
Clean tubes:
Situation 1, when test finish, you have done all the test. Wash tube for next day test.
A. When do the test, choose “Draining”.
B. Select “Lift wash” method. Set wash times “3”. Do not choose dry wash.
C. Test finished, result is true. The machine will discharge the testing sample automatic.
D. Fill in the solvent into the tube through Sand core funnel.
E. Click start, the machine will wash the tube 3 times, and discharge the waste liquid when wash finished.
F. Fill in the Ethanol, or acetone into the tube through sand core funnel.
G. Select “Lift wash” method. Set wash times “3”. Set the dry wash time 600s.
H. Machine will wash the tubes automatic and discharge the waste liquid, then drying 10 minutes.

Situation 2, when A sample test finished, go B sample test.

Use half of the B sample for washing, half of B sample testing.
A. When do test, choose “Rinse” and “Draining”.
B. When A sample test finished, the result is true, the will discharge the waste liquid.
C. Then software will remind you to fill the half of sample B.
D. Fill the sample B through Sand core funnel, and click confirm.
E. Machine will wash the tubes 3 time (time can be set on the method) by using sample B.
F. When wash finished, it will discharge the waste liquid, and remind you to fill sample B.
G. Fill the rest of sample B, and confirm, it will start the test, and show result.
When tube is suspected dirty (water goes into the tube) or something inside the tubes. (Only do in the Fume Hood!!!)
1. Heavy wash. Take out the tubes, and using the 98% concentrated sulfuric acid to fill into the tube, and place it for 24 hours.

2. After 24 hours, pour out the concentrated sulfuric acid. Fill in the water inside tube for wash by hand ( use the water to bring out the acid).
3. Pour out the water, and fill the ethanol to wash. (ethanol can bring out the water, and easy to volatilize, so can keep tube dry).
4. If possible, use a pump machine to send air to keep tube drying. Or place the tube in the oven ( below 100 ℃, 30 minutes).