GB/T 27846-2011 Determination of chemical viscosity by Hoppler falling ball viscometer method GB/T27846-2011 Standard compression package decompression password: www.bzxz.net
This standard specifies the method for determining the dynamic viscosity of Newtonian liquids using the Hoppler falling ball viscometer. This standard is applicable to the measurement of dynamic viscosity in the range of 0.6mPa·s~250000mPa·s at temperatures of -20℃~120℃.
class="f14" style="padding-top:10px; padding-left:12px; padding-bottom:10px;"> This standard was drafted in accordance with the rules given in GB/T1.1-2009.
This standard has the same technical content as the German standard DIN53015:2001 "Viscosity Determination by H.ppler Falling Ball Viscometer Method" (English version).
This standard has been edited as follows:
———The foreword, revision and previous version of the German standard have been deleted;
———"References" have been added.
This standard was proposed and managed by the National Technical Committee for Hazardous Chemicals Management Standardization (SAC/TC251). The
drafting units of this standard are: China Institute of Inspection and Quarantine, China Chemical Economic and Technological Development Center, Jiangsu Coal Chemical Engineering Design and Research Institute Co., Ltd., and Sinochem Chemical Standardization Research Institute.
The main drafters of this standard are: Sun Xin, Chen Huiming, Wang Xiaobing, Yang Ting, and Guo Xinyu.
The following documents are indispensable for the application of this document. For all dated referenced documents, only the dated version applies to this document. For any un-dated referenced documents, the latest version (including all amendments) shall apply to this document.
ISO/TR3666 Viscosity of water
DIN1319-1 Fundamentals of metrology—Part 1: Basic terminology
DIN1319-3 Fundamentals of metrology—Part 3: Evaluation of measurements of single measurement values ​​and measurement uncertainty
DIN1342-1 Viscosity—Part 1: Rheological concepts
DIN12785 Laboratory glassware; special purpose laboratory thermometers
DINISO3585 Borosilicate glass 3.3 Borosilicate glass 3.3—Properties
ISO/IEC Guide 98 Guide to the expression of uncertainty in measurement

ICS 13.300
National Standard of the People's Republic of China
GB/T 27846-2011
Chemicals-Measurement of viscosity using the Hoppler failing-ball viscometer
Chemicals-Measurement of iscosity using the Hoppler failing-ball viscometer2011-12-30 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Administration of Standardization of the People's Republic of China
Implementation on August 1, 2012
This standard was drafted in accordance with the rules given in GB/T 1.1-2009. CB/T 278462011
This standard has the same technical content as the German standard DIN 53015:2001 "Determination of viscosity using the Hoppler falling-ball viscometer" (English version).
This standard has been revised as follows:
The foreword of the German standard has been deleted, and the revision and previous version: - "References" have been added.
This standard is proposed and managed by the National Technical Committee for the Management of Hazardous Chemicals (SAC/TC251). The originators of this standard are: China Institute of Inspection and Quarantine, China Chemical Economic and Technological Development Center, Jiangsu Coal Chemical Engineering Design and Research Institute Co., Ltd., and Sinochem Chemical Standardization Research Institute. The main drafters of this standard are: Sun Xin, Chen Huiming, Wang Xiaobing, Yang Ti, and Guo Xinzi. I
TTTKANTKACA
Determination of chemical viscosity Hoppler
Falling ball viscometer method
This standard specifies the method for determining Newtonian dynamic viscosity using the Hoppler falling ball viscometer. GB/T 27846-2011
This standard is applicable to the measurement of dynamic viscosity in the temperature range of -20℃~120℃F 0,6 mPa~250 000 mPa s. Normative references
The following documents are indispensable for the application of this document. For any dated referenced document, only the version with the previous date is applicable to this document. For any un-dated referenced document, the latest edition (including all amendments) applies to this document. ISO/TR 3666 Viscosity of water DIN 1319-1 Fundamentals of measurement technology - Part 1: Basic terms DIN 1319-3 Fundamentals of metrology - Part 3: Measurement of single measured values, evaluation of measurement errors DIN 1342-1 Viscosity - Part 1: Rheological concepts DIN 12785 Laboratory glassware special purpose laboratory thermometers DIN IS() 3585 Borosilicate glass 3.3 Properties 1SO/IEc Guide 98 Guide to the expression of uncertainty in measurement
3 Terms and definitions
The terms and definitions defined in DIN 1319-1 and DIN V 1342-1 and the following terms and definitions apply to this document. 3. 1
Standard viscosity test sample sample is a standard Newtonian liquid sample whose viscosity is measured at one or more temperatures using a standard viscometer. Its viscosity value and traceability are recorded in the national viscosity standard and used as a physical measuring tool for publishing viscosity units. 4 Symbols, quantities and units
Symbols, quantities and units are shown in Table 1.
Table 1 Symbol Quantity and Unit
Sphere Diameter
Difference between Sphere and Liquid Density
TTKNTKACA
SI Unit
Other Legal Units
GB/T 27846--2011
Ie, +tai?
Acceleration due to gravity at the viscosity measurement site Table 1 (continued)
Acceleration due to gravity at the viscosity measurement site Acceleration error due to gravity at the viscosity measurement site
Mass of the sphere
Weight of the sphere mass disk
Number of drops in a series of measurements
Relative variance of the density difference between the sphere and the liquid
Relative variance of the calibration constant
Relative variance of the viscosity due to the deviation of the viscosity ratio from the horizontal
Relative variance of the sphere falling time
Relative force difference of the timer
Standard deviation of the viscosity measurement
Viscosity due to uncertainty in the temperature measurement Relative variance Variance of liquid density
Variance of sphere density
Relative variance of sphere density
Falling time of sphere
Shortest falling time required for calculation of uncertainty (see Table 4) Shortest falling time for calculation of repeated measurements The longest and shortest falling time of sphere in a series of single measurements
Uncertainty of temperature coefficient of viscosity
Temperature coefficient of dynamic or kinematic viscosity
Relative uncertainty of viscosity measurement
Relative uncertainty of sphere density value Relative uncertainty for determination of calibration constantbzxz.net
Air buoyancy zone number
SI unit
Pa-s- n'/(kg+s)
kg*/m*
kg /me
TTTKNTKACA
German legal unit
mPa-s+cm'/(gs)
g\ /en
Coefficient of linear thermal expansion
Table 1 (continued)
Relative range of the falling time of a sphere in a series of measurements using a viscometer
Dynamic viscosity
Dynamic viscosity of the standard sample
Dynamic viscosity of the standard sample at the reference temperatureTemperature
Calibration temperature
Body density
Body density
Guideline value of sphere density (for calculation of air buoyancy correction) 5 Measuring range
SI unit
GB/T 27846—2011
Other statutory units
mPa·s
This standard is suitable for measuring dynamic viscosities in the range of 0.6 mPa·s to 250,000 mPa·s at temperatures between -20°C and 120°C. To cover this range, six balls of different diameters should be used, each covering a portion of this range (see Table 2). NOTE 1: If the density of the liquid to be measured is 1.0 g/cm3 or more, the lower limit of 0.6 mPa·s is reached at the shortest drop time specified in Table 3. NOTE 2: If the materials used (e.g. seals, water supply hoses) are suitable, it is possible to measure outside the specified temperature range (-40°C to 150°C). The difference between the temperature measured in the heat pipe sleeve and the temperature of the drop pipe specimen may be greater than the temperature specified in 8.4. Table 215. Viscometer sphere diameters corresponding to an internal drop of 94 mm diameter Sphere No.
Borosilicate glass
Borosilicate glass
Inlaid/Iron
Nickel/Iron
Gold/Iron
Nickel/Iron
Density (guideline value) p/
(g/cm*)
Sphere diameter/
15. 81+0. 01
15.6±0.05
15.6±0.05
15. 2±0. 1
14. 0±0.5
Difference in value/
±0. 000 5
±0.000 5
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Calibration constant (guidance value) K/
mPa- s- cm'/(gs)]
Viscosity measuring range/
(mPa-s)
40-700
150~5 000
1 500~50 000
7 500 and above
CB/T 278462011
6 Principle
The time required for a sphere under the action of gravity to travel a distance marked with a mark (gauging length) is measured in an inclined circular tube filled with test liquid.
7 Calculation method
The kernel method uses the viscosity formula obtained from the new Stokes law, see formula (1): -K×(Px-Pp)Xt×
Note, the band number and (are determined by calibration (now Chapter 11). 8 Instruments
8.1 Hoppler falling ball viscometer
++++++++( l )
8.1.1 The viscometer (see Figure 1) consists of a drop tube filled with the liquid to be tested and a sphere selected to suit the viscosity of the liquid. The drop tube is surrounded by a thermal control sleeve (referred to as "heat sleeve") mounted on a frame. The heat sleeve and the drop tube are connected together by a pivot, which is perpendicular to the axis of the drop tube and tilted to the horizontal direction at an angle of 10±1. When the sphere returns to the starting position, the drop tube and heat sleeve assembly can be rotated 180° relative to the frame. In the starting position, the assembly is fixed to the frame by a locking device. The frame has three legs, two of which are The height can be adjusted by means of leveling screws. There is a level with a maximum error of 0.2\ on the stand, which ensures that the drop tube is at the correct angle in the vertical direction. The temperature is measured in the heat pipe sleeve with a replaceable thermometer. 8.1.2 The drop tube\ is a precisely calibrated glass tube made of borosilicate glass 3.33 according to DINISO3585. Borosilicate glass has a linear thermal expansion coefficient of 3.3×10-K-1 and an inner diameter of 15.94 mm. There are two upper and lower marks (M, and M, respectively) in the middle section of the drop tube to determine the measuring length (100 mm ± 1 mm), in addition to a drop tube identification number and a vertical line or class mark. The drop tube is to be inserted so that the arrow on the heat pipe jacket cover is aligned with the vertical line. The drop tube is sealed with two plugs, the upper of which has a capillary connected to a cavity. The purpose of the two plugs is to prevent unacceptable changes in pressure and air ingress when the temperature fluctuates.
8.1.3 All 6 spheres of the viscometer, each of which is ensured to be within the measurement range given in Table 2. All spheres should share the same linear thermal expansion coefficient as the drop tube (i.e. 3.3×10-°K-\), otherwise the uncertainty method cannot be applied: 8.2 Thermometer
As long as the full manifold and the correction value specified in the calibration certificate are used, the temperature inside the heat pipe jacket is allowed to fluctuate. The uncertainty of the measurement is 0.03° (see Chapter 12), then either a calibrated (fully immersed) mercury-in-glass thermometer or an electrical thermometer may be used. Suitable thermometers are, for example, DIN 12785 mercury-in-glass thermometers designed to comply with the Höppler viscometer or appropriately designed pin resistance thermometers. If the uncertainty of the measured value of the temperature measurement in the tube sleeve is greater, then the tolerance should be calculated in the uncertainty calculation of 12.2. The thermometer should be protected from thermal radiation during the measurement. 1) This terminology adopts RS188. Reference is made to the "measuring tube" in the international standard ISO12058-1. 2) The ball with certain chemical resistance and physical properties specified in DLVIS09585 is called *silicon glass 3.3F. 4
TTTKAONYKACA
Heat pipe sleeve:
Drop pipe:
Ball:
Seat frame;
Pivot:
Locking device;
Leveling screw;
Level:
Thermometer:
Mark.
Figure 1 Example of Hoppler falling ball viscometer
GB/T27846—2011
Unit is mm
GB/T 278462011
8,3 Timer
The timer should be a stopwatch with a reading accuracy of 0.01. It should be recalibrated after a period of time according to its model and working conditions, and pay attention to ensure that the relative uncertainty of the measured value does not exceed 2×10-. 8.4 Thermostat
The thermostat used shall be an automatically controlled thermostatic bath connected by a closed circuit to the thermowell of the viscometer and shall ensure that the temperature in the thermowell varies within 0.02°C from 10 to 70°C (or within 0.05°C when the temperature is outside this range) during a series of measurements.
After the specified time has elapsed since steady-state conditions were reached, the indicated temperature in the thermowell shall not differ from the temperature in the drop tube by more than 0.01°C. 8.5 Density measurement
The density shall be measured by an instrument capable of determining the density of the liquid under test with the following relative uncertainty of measurement: a) 5 × 10* if a glass sphere is used; b) 1 × 10* if a gold sphere is used. NOTE Suitable instruments are, for example, the vibrating densitometer of ISO 12185 and ISO 15212.1, or the hydrometer combined with a balance of ISO 3507. 9 Sampling
A viscometer is filled with approximately 40 ml of sample. The sample should be collected and pre-treated in accordance with the requirements of the liquid to be tested or in accordance with the relevant standards for sampling of the test fluid. 10 Preparation
10.1 Preparation of the Sample
10.1.1 If the sample has been prepared in accordance with the provisions of Chapter 9, no further preparation is necessary. However, high-viscosity liquids may need to be heated before being added to the viscometer if the viscosity of the liquid remains unchanged when heated and then returned to the measurement temperature. NOTE: If the measurement is made when the liquid or its components are close to the freezing point, non-Niuwei characteristics may appear. 10.1.2 Unless otherwise specified, the sample shall only be filtered if particulate matter in the liquid affects the measurement. In this case, the diameter of the filter used shall be stated in the test report. Hazardous substances should be handled in accordance with occupational safety regulations and relevant regulations on waste disposal.
10.2 Selection of spheres
10.2.1 The drop time of the selected sphere should not be less than the value listed in Table 3. Table 3 Shortest drop time
Shortest drop time/
Sphere number
Qiu 3 (continued)
Shortest drop time:
GB/T 27846—2013
10.2.2 In Table 3, 1 is the shortest drop time required to calculate the uncertainty (see Table 4) according to 12.2, and t is the shortest drop time to obtain repeatable measurements. A drop time less than 1 will cause a systematic deviation (i.e., a longer transfer time) in formula (1)), which can reach several percent. The calibration curve of each viscometer can be determined using some bodies of known viscosity. 10.3 Measurement of the falling time
10.3.1 Preparation of the apparatus
10.3.1.1 Clean the viscometer sphere, the end caps and cover plates of the drop tube, the plug and the seal with a suitable liquid and the drop tube cleaning caps provided. Before calibration, first clean them with volatile petroleum ether without residue (or, for example, disinfectant alcohol for cleaning as specified in the German Pharmacopocia). After rinsing several times, dry them in an oven at a temperature of no more than 10 000 °C. 10.3, 1.2 Ensure that the capillary on the plug is not blocked. 10.3.1.3 Before measuring, protect the sphere, drop tube, end caps and cover plates, plug and seal from dust. 10.3.1.4 Insert the drop tube so that the arrow on the shrink-fit cover is aligned with the longitudinal line of the drop tube or the mark on the drop tube. 10.3.2 Procedure
10.3.2.1 Calibrate the viscometer using the built-in level and then place the sample into the drop tube as specified in the viscometer operating manual. After the temperature stabilizes for 30 minutes, remove the upper end cap and then reinstall and tighten it to form a pressure balance. Ensure that air is fully introduced into the tube.
10.3.2.2 Turn the drop tube 180° and allow the ball to fall to the starting position. After heating, turn the drop tube 180° again and measure the time required for the ball to move from the upper timing mark to the lower timing mark. Observe these marks with a magnifying glass to avoid parallax. Start the measurement when the lowest point on the outer surface of the ball passes through the upper timing mark and aligns with the virtual plane. Stop the measurement when it passes through the lower timing mark and aligns with the virtual plane. Measure the falling time 5 times.
10.3.2.3 If the liquid is opaque, the sphere will be indicated by a bright spot on the tube wall. In this case, use the Yao point to determine the time through the two marked channels.
10.3.2.4 Read the temperature immediately before and after the measurement. Ensure that the difference between the highest and lowest temperatures does not exceed 0.02°C. 10.3.2.5 Calculate the average of the five falling times and check the relative difference between the longest and shortest falling times, see equations (2) and (3) 5, = m = ≤2.0 ×10-
E, ≤ 2.5 ×10 3 ...
GB/T 27846—2011
10.3.3 Measurement of liquid density
Determine that the measurement accuracy of the liquid density meets the requirements of 8.5. 10.4 Evaluation of results
10.4.1 Calculate the dynamic viscosity in mPa·5 using equation (1) in Chapter 7, replacing t with the average falling time and replacing the sphere and liquid density values ​​with the density values ​​at the time of temperature measurement. 10.4.2 Assuming that the calibration has been carried out in accordance with the provisions of this standard and the relative uncertainty of the sphere band number is consistent with the value specified in Table 6, if the requirements specified in Chapters 8 to 10 are met, the falling time is not less than 4 in Table 3, and P, is equal to 0.8 g/cm, then the relative uncertainty of the dynamic viscosity measurement value given in Table 4 shall be used. The temperature coefficient of viscosity is 0.07 K for spheres 1 to 4 and 0.1 K-110 for spheres 1,5 to 6. 4.3 If a calibrated (fully immersed) DIN 12785 mercury-in-glass thermometer with a scale interval of 0.1 °C and an uncertainty in the measured value of 0.1 °C or another thermometer with a similar uncertainty is used, and the determination is made by total immersion and only three, instead of five, sphere drops, the uncertainty of the measured value specified in Table 4 shall be increased by 0.1 % for spheres 1 to 4 and by 0.6 % for spheres 5 and 6. Table 4 Relative uncertainty u, of the dynamic viscosity measurement value when the slow determination meets the requirements of Chapters 8 to 10, the liquid density P, is 0.8 g/cm and the falling time is not shorter than t, listed in Table 3 (applicable to K= 2) Sphere number
Relative uncertainty u, of the viscosity measurement value /%
10.4.4 If the measurement conditions are different, the uncertainty shall be evaluated according to the provisions in Chapter 12. 10.5 Test report
The test report shall refer to this standard and include at least the following contents: a> Identification of sample material:
b) Measurement temperature, in degrees Celsius (℃); e)
The sphere number, drop tube number, sphere band number and sphere density at 20 ℃ used; the dynamic viscosity of spheres No. 1 to 4 shall be 4 significant figures, and the dynamic viscosity of spheres No. 5 and 6 shall be 3 significant figures, in d
milliPascal seconds (mPas);
Uncertainty of the measurement value of dynamic viscosity:
The correction value adopted;
Measurement date.
11 Viscometer calibration
11.1 Principle
The principle of viscometer calibration includes: the calibration of the viscometer (e.g. by the manufacturer, the user or an authorized laboratory), the repeatability of the results8
GB/T 27846-—2011
and the uncertainty of the measurement value evaluated in accordance with Clause 12. Calibrate each required sphere and include the following: a) Measure the diameter and mass m of the sphere and calculate the density of the sphere using formula (4): x
Use formula (5) to determine the sphere constant K from the falling time of the sphere using two standard samples with known viscosity holes but different densities:
11. 2 Standard samples and instruments
The following standard samples and instruments should be used:
(P-PN)X
Select two standard samples with different viscosities so that the relative uncertainty of the falling time and the measured value meets the requirements specified in Table 5. The density of the standard sample should be in the range of 0.8 g/cm~1.2 g/cm*, with a relative uncertainty not exceeding 5×10-*. A balance suitable for determining the mass of the sphere should have an accuracy of 0.2 mg. If necessary, use a standard magnetic code for calibration: The glass water thermometer suitable for the falling ball viscometer has a measuring range of 19°C~21°C and a scale interval of 0.02 ℃ (e.g. DIN12785 thermometer) + full immersion calibration + with specified correction value, uncertainty does not exceed 0.01℃. As long as the measurement uncertainty of the thermometer does not exceed 0.1℃, a calibrated suitable electric thermometer (e.g. platinum resistance thermometer) can be used. t
Device and measuring speed for measuring the diameter of the sphere, with a resolution of 0.2μm and an uncertainty of 0.00002m (e.g. an outside micrometer with a vernier scale interval of 0.002mm):
Timer in 8.3;
Thermostat in 8.4.
Standard specimen for calibrating the viscometer
Sphere guide
11, 3Calibration conditions
Falling time during calibration/
700~800
900~1000
300--400
500--600
300-400
500600
300--400
50~600||t t||300~~400
500~600
300--400
500-600
The conditions suitable for calibration are as follows
Viscosity guide value/
(mPa·s)
200-270
330--400
1500~2 100
2 300-~3 100
15 00020 000
25 000-~30 000
75 000--100 000
125 000 ~150 000
Relative uncertainty of maximum allowable viscosity
(for K=2)
GB/T27846—2011
a) Ambient temperature: 20±1℃
b) Temperature in the viscometer tube sleeve; 19. 9℃～20. 1℃; the allowable temperature change in the tube sleeve during multiple measurements is ≤0.02 d Temperature of the ball in diameter measurement: 20 ±1 ℃; Time for the standard sample in the viscometer to reach thermal equilibrium: 30 min inclusive; e)
Time for the sphere to reach thermal equilibrium before measuring the diameter: ≥3 h; g) Time from filling the viscometer to the end of the drop time measurement: ≤6 h. 11.4 Number of measurements
11.4.1 When determining the sphere constant, each sphere and each two standard samples of different viscosities need to be dropped 5 times for measurement (see 11.2). 11.4.2 The diameter of the sphere should be measured at 10 different points on the surface that are as evenly distributed as possible. 11.5 Cleanliness and finish
All viscometer parts should be kept clean and should not have any visible defects that may affect the function (such as scratches on the inner wall of the drop or on the surface of the sphere).
11.6 Determination of sphere density
11.6.1 Mass of sphere
The mass of the sphere shall be calculated using equation (6) in grams (g): m=W
where:
Pkw-1.2×10-1
0.999850XPxw
Note: When using equation (7) to calculate the air elastic correction value, replace the sphere density value P1 with the appropriate guide value in Table 2. 11.6.2 Diameter of sphere
(7)
11.6.2.1 The sphere shall be removed only with the aid of tools (e.g., tweezers) to prevent contamination and temperature changes. The manufacturer's instructions for measuring and assembling the sphere shall be followed during the measurement. The force exerted by the measuring device on the sphere shall not exceed 1 N to prevent the sphere from being crushed (Hertzian pressure). 11.6.2.2 The deviation from roundness should not be greater than 0.5 μm for spheres 1 and 2, 1 μm for spheres 3 to 5, and 2 μm for sphere 6.
11.6.3 Sphere density
The mass of the sphere is calculated using equation (6), and the density of the sphere is calculated using equation (4) by the average value of the ten sphere diameters and the sphere mass. 1.7 Determination of sphere constant
11.7.1 Prepare for the measurement and determine the ball falling time as specified in 10.3. Calculate the calibration constant from the dynamic viscosity of the standard sample at the calibration temperature, the average value of the ball falling time and the ball viscosity using equation (5). 11.7.2 If the calibration temperature does not differ from 20 °C by more than 0.1, convert the viscosity of the standard sample at 20 °C to the viscosity at the calibration temperature using equation (8):
7mg = m[1 +U,(20 -k)]
++++( 8)
Note: U, can be found on the calibration certificate of the standard sample (U, can be set equal to Uv). See Table 6 of the uncertainty of calibration measurements in 12.3. 10
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