17.2 Qualitative Determination of Starch in Water-Soluble Polymers
17.2.1 Principle
17.2.1.1 The purpose of this test is to determine the presence of starch or starch derivatives in powdered or granular water-soluble polymers such as PAC-LV
17.2.1.2. Detection of PAC-LV solution by adding a mineral/iodide solution*
If amylose is present, it is rendered into a colored complex.
17.2.2 Reagents and materials
a) Deionized or distilled water
b) Nitrate solution, eg Merck 1.09.089.1000 (CAS No. 7553-56-2) 7) 0.05.
c) Potassium iodide 1 Merck 1.0504 3.0250 PA (CAS No. 7681-11-0
d) Sodium hydroxide (NaOH) (CAS No. 1310-73-2): dilute solution, 0.1%-0.5%.
17.2.3 Apparatus
17.2.3.1 Stirrer 1ta Model 98 Multi-shaft Stirrers equipped with a 9B29X impeller or equivalent blade with a single
sinusoidal waveform, blade diameter approx. 25 mm (lin, punched face up).
17.2.3.2 The agitation cup has an approximate size of 180 mm (7.1 in) deep, 97 mm (3-5/6 in) diameter of the
upper mouth, and 70 mm (2.75 in) diameter of the lower base (eg M110-D type Hamilton Beach stirring cup
or equivalent Thing). (A 600 ml glass can also be used as a substitute.)
17.2.3.3 Laboratory spoons.
17.2.3.4 Scraper.
17.2.3.5 Balance: The accuracy is 0.01 g.
17.2.3.6 Volumetric flasks 100ml
17.2.3.7 Pasteur pipettes or dropper plastics.
17.2.3.8 Timer: Mechanical or electronic, accuracy 0.1 min. 17.2.3.9 pH meters and pH electrodes:
eg Thermo Russell type KDCW1 19)
17.2.3.10 Polymeric feeding devices (eg Fann 10) or 0Fl type 11))
17.2.3.11 Test tubes.
17.2.4 Procedure - Preparation of Iodine/Potassium Iodide Solution
17.2.4.1 Add 10 μl ± 0.1 ml of 0.05 mol / l iodine solution to a 100 ml ± 0.1 ml volumetric flask.
17.2.4.2 Add 0.60 g±. .01 g Potassium iodide (KI), gently shake the flask to dissolve it.
17.2.4.3 Add deionized water to a 100 ml mark and mix thoroughly. Record the date of preparation.
17.2.4.4 The formulated iodine/iodide solution is stored in a closed container and stored in a dark, cool and dry place.
The expiration date is up to three months and should be discarded and reconstituted.
17.2.5 Procedure - PAC-LV Solution Preparation and Starch Detection
17.2.5.1 Prepare a 596 aqueous solution of PAC-LV to be tested.
Add 380 g ± 0.1 g of deionized water to the mixing cup, add 2 g ± 0.1 g of PAC-LV at a uniform speed
while stirring on the stirrer, and the addition time should continue for 60 s to 120 s.
The sample should be added to the turbulence in the mixing cup, and avoid stirring shaft to reduce dust.
It is preferable to use the polymer charging device in 17.2.3.10.
17.2.5.2 After stirring for 5 min ± 0.1 min, remove the stir cup from the stirrer and scrape all PAC-LVs stuck to
the cup wall with a spatula. All PAC-LVs stuck to the scraper were mixed into the solution.
17.2.5.3 Measure the pH of the solution. If the pH is lower than 10, add a dilute solution of NaOH dropwise.
Raise the pH to 10
17.2.5.4. Return the stirring cup to the stirrer and continue stirring. The total stirring time should be 20 min ± 1 Min.
17.2.5.5 Place 2 ml of the sample solution into a test tube and add dropwise 3 drops of iodine/iodide solution,
up to 30 drops.
17.2.5.6 Prepare three blank assays with deionized water. Add 3 drops, 9 drops, 30 drops of iodine/iodide solution to
the tubes for comparison tests.
17.2.5.7 After adding 3 drops of solution each time, gently shake the tube to compare the color of the sample solution
with the blank test. The comparison of colors should be made against a white background.
17.2.6 Determination - PAC-LV Starch Detection
17.2.6.1 If the sample solution to be tested exhibits the same yellow color as the blank test, the sample does not
contain any starch or starch derivatives.
17.2.6.2 If any other color is present, it is strongly indicated that there is a starch or starch derivative
17.2.6.3 If the color appears to disappear quickly, indicating the presence of a reducing agent, in this case,
continue to add dropwise iodine / iodide Solution, color comparison with one of the blank tests, see 17.2.61.
17.2.6.4 If any color reaction that is different from 17.2.6.1 is detected, it is not necessary to proceed with the next test
17.3 Moisture
17.3.1 Apparatus 17.3.1.1 Oven: Controllable at 105°C±3°C (220±5>.
17.3.1.2 Balance: Accuracy of 0.01 g.
17.3.1.3 Evaporation dish: Capacity 150 ml.
17.3.1.4 Scraper.
17.3.1.5 Desiccator: Contains desiccant (CAS No. 7778-18-9) desiccant, or equivalent
17.3.2 Test Procedure
17.3.2.1 Weigh 10 g ± 0.1 g PAC-LV sample to weighed In the evaporating dish, record the sample mass m
17.3.2.2 Dry the sample in the oven for 4 h
17.3.2.3 Cool the sample in a desiccator to room temperature17.3.2.4 Reweigh the evaporating dish containing the
dried PAC-LV , record dry sample quality m2.
17.3.3 Calculation
17.4 Fluid loss
17.4.1 Reagents and materials
17.4.1.1 Sea salt: Evaluate soil according to ASTM D 1141-98 (2003) 12
17.4.1.2 API standard.
17.4.1.3 Potassium Chloride (CAS No. 7447-40-7)
17.4.1.4 Sodium Bicarbonate (CAS No. 144-55-8).
17.4.1.5 Deionized or distilled water.
17.4.2 Instruments
17.4.2.1 Thermometer: The measuring range is 0 °C ~ 60 °C, the precision is 0.5 °C
(the measuring range is 32 °F ~ 140 °F, the precision is 1.0 °F)
17.4.2.2 The balance: The precision is 0.01g.
17.4.2.3 Stirrer: If a Type 9B multi-shaft stirrer is equipped with a 9B20x impeller, the shaft should be fitted with a
single sine wave blade with a blade diameter of approximately 25 mm (1 in) with a stamped face up.
17.4.2.4 The agitation cup has an approximate size of 180 mm (7.1 in) deep, 97 mm (3-5/6 in) diameter of
the upper mouth, and 70 mm (2.75 in) diameter of the lower base (eg M110-D type Hamilton Beach stirring cup).
17.4.2.5 scraper.
17.4.2.6 Container: Glass or plastic, with a stopper or lid, used for salt water.
17.4.2.7 Viscometers: Electric, direct reading, in accordance with ISO 10414-1
17.4.2.8 Timers: Two, mechanical or electronic, with a precision of 0.1 min for the time period measured in this test.
17.4.2.9 Filtration Apparatus: Low temperature and pressure type, in accordance with the provisions of Chapter 7 of
ISO 10414-1:2008.
17.4.2.10 Measuring cylinders: Two, with a capacity of 10 ml ± 0.1 ml and 500 ml ± 5 ml *
17.4.2.11 Polymer feeding device (Fann type or OFI type).
17.4.3 Test Procedure - PAC-LV Fluid Loss
17.4.3.1 Add 42 g ± 0.01 g of sea salt to 11 ± 2 ml of deionized water.
17.4.3.2 In 358 g of sea salt solution, add 35.0 g ± 0.01 g of potassium chloride (KCl).
17.4.3.3 After stirring for 3 min ± 0.1 min, add 1.0 g ± 0.01 g of sodium bicarbonate.
17.4.3.4 After stirring for 3 min±0.1 min, add 28.0 g±0.01 g API standard to evaluate
17.4.3.5 After stirring for 5 min±0.1 min, remove the stirring cup from the stirrer and scrape it to the wall with a scraper.
All API standards evaluate soil. All API standard evaluation soils stuck to the scraper were mixed into the suspension.
17.4.3.6 Return the stirring cup to the stirrer and continue stirring for 5 min ± 0.1 min.
17.4.3.7 Weigh 2.0 g±0.01 g PAC-L.
17.4.3.8 Slowly while stirring on the stirrer, add PAC-LV at a uniform rate.
The addition time should last approximately 60 seconds. The PAC-LV should be added to the vortex in the mixing cup
and avoid the stirring shaft to reduce dust. It is best to use the polymer feed device in 17.4.2.11.
17.4.3.9 After stirring for 5 min ± 0.1 min, remove the stir cup from the stirrer and use a spatula to scrape off all
PAC-L stuck to the cup wall. All PAC-LVs stuck to the scraper were mixed into the suspension.
17.4.3.10 Return the jar to the stirrer and continue stirring. If necessary, after 5 minutes and 10 minutes, remove the stir
cup from the stirrer and scrape off all PAC-L stuck to the cup wall. The total stirring time from the
start of addition of PAC-LV should be 20 min ± 1 min.
17.4.3.11 At 25 °C ± 1 °C (77 °F ± 2 °F), maintain the suspension in a closed or lidded container for 16 h ± 0.5 h.
Record curing temperature and curing time.
17.4.3.12 After curing, stir the suspension on a stirrer for 5 min ± 0.1 min.
17.4.3.13 Pour the PAC-LV suspension into the filter cup. Before pouring into the suspension, make sure that all parts
of the filter cup are dry and the seal ring is not deformed or worn. The temperature of the suspension should be
25°C±1°C (77°F±2). To within 13 mm (0.5 in) from the topof the cup. Assemble the filter cup, install the filter cup on
the holder, close the pressure relief valve, and place a container under the drain tube.
17.4.3.14 Set a timer to 7.5 min and another set to 30 min. Simultaneously start two timers and adjust cup pressure to
690 kPa ± 35 kPa (100 psi ± 5 psi). The pressure should be provided by compressed air, nitrogen or helium.
It should be completed within 15 seconds.
17.4.3.15 at first At the end of the timer only, remove the container and remove any liquid adhering to the drain and
discard it. A dry 10 ml graduated cylinder was placed under the drain and the filtrate was collected until the second
timer expired. Remove the cylinder and record the volume of filtrate collected.
17.4.4 Calculation - Loss of PAC-LV The amount of filtrated V is calculated according to equation (43) in ml;
v-2xVe (43) where: 1⁄2_ volume of filtrate collected between 7.5 min and 30 min. The unit is ml.
17.5 Apparent Viscosity of Solutions
17.5.1 Test Procedure - Apparent Viscosity of Solution
17.5.1.1 Add 42 g ± 0.01 g of sea salt to 11 ± 2 ml of deionized water.
17.5.1.2 In 358 g of sea salt solution, add 35.0 g ± 0.01 g of potassium chloride (KCl).
17.5.1.3 Weigh 5.0 g ± 0.01 g PAC-Lv. Slowly while stirring on the stirrer, add PAC-LV at a uniform rate.
The addition time should last approximately 1 minute. The PAC-LV should be added to the vortex in the mixing cup
and avoid the stirring shaft to reduce dust.
17.5.1.4 After stirring for 5 min ± 0.1 min, remove the stir cup from the stirrer, scrape all PACw stuck to the cup wall
with a spatula, and mix all the PAC-LV stuck on the spatula to the suspension.
17.5.1.5 Return the jar to the mixer and continue stirring. If necessary, remove the stirrer cup from the mixer after
5 min and 10 min, scrape all PAC-Ws stuck to the cup wall. The total stirring time from the start of addition of
PAC-LV should be 20 min ± 1 min.
17.5.1.6 At 25 °C ± 1 °C (777 ± 27), suspend the suspension for 16 h ± 0.5 h in a closed or lidded container.
Record curing temperature and curing time ”
17.5.1.7 Stir the suspension on the stirrer for 5 min ± 0.1 min.
17.7.5.1.8 Pour the solution into the sample cup equipped with a direct reading viscometer” at 25 °C ± 1 °C (77 Under
the condition of °F ± 2), the suspension was read at 600 r / min.
17.5.2 Calculation - Apparent viscosity of the solution
Calculate the apparent viscosity of the solution according to formula (44), in mPas:
VA=R600/2 (44)
R600-viscometer reading at 600 r / min. Record the result of calculation
Post time: Nov-12-2020