Some standard content:
ICS 71. 100. 30
National Standard of the People's Republic of China
GB/T9107—1999
Refined cotton
Refined cotton
Published on September 10, 1999
Implemented on April 1, 2000
Published by the State Administration of Quality and Technical Supervision
GB/T 9107 1999
Cited standards
Product classification and code
Test methods
Inspection rules
Marking, packaging, transportation, storage
Appendix A (Appendix to standards) Standards of raw materials cited in this standard Appendix B (Appendix to standards)
4 (Appendix to suggestions)
Appendix work (Appendix to suggestions)
Preparation method of copper ammonia solution
Corresponding measurement values of degree of polymerization and viscosity
Determination method of degree of polymerization
GB/T 9107 --1999
This standard is a revision of GB/T9107--1988% refined cotton based on the needs of the development of the market economy and my country's national conditions. The main technical differences between this standard and GB/T9107-1988 are: adding product models; making specific provisions for physical and chemical performance items and index requirements according to product use. This standard will replace GB/T9107-1988 from the date of implementation. Appendix A and Appendix B of this standard are supplementary appendices. Appendix C and Appendix D of this standard are indicative appendices. This standard is proposed by China Ordnance Industry Corporation. This standard is under the jurisdiction of China Ordnance Industry Standardization Research Institute. The originating units of this standard are Xi'an Hui'an Chemical Plant and China Ordnance Industry Standardization Research Institute. The main drafters of this standard are Zhu Xingcai, Tu Ligang, Yang Jinxia, Xing Bing, Wang Ping, and Zhang Luli. This standard was first issued in April 1988.
1 Scope
National Standard of the People's Republic of China
Refinerl cotton
GB/T 9107
Replaces GB/T 9107 --1988
This standard specifies the classification, requirements, test methods, inspection rules and marking, packaging, transportation, storage, etc. of refined cotton. This standard is applicable to refined cotton made from cotton linters after alkali boiling, bleaching and other refining treatments. 2 Cited Standards
The texts contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are all current: All standards will be revised. Parties using this standard should explore the possibility of using the latest versions of the following standards: B/T603-1988 Preparation of preparations and products used in chemical reagent test methods B/T 8170-1987 Rules for numerical rounding off
The raw material standards cited in this standard are shown in Appendix A (Annex to the standard) 3 Product classification and code
3.1 Products are divided into three categories according to their use, namely, refined cellulose for cellulose acetate, nitrocellulose and cellulose cellulose 3.2 Product codes are generally composed of use codes, specification codes and performance codes, and their display method is shown in Figure 1. Performance code
Specification code
Use code
Figure 1 Product code representation method
32.1 The use code indicates the use of the product, with a capital letter for each letter, see Table 1. Table 1 Usage code for refined sugar
For cellulose acetate
For nitrocellulose
Specification code indicates the specification of the product, taking the middle value of the viscosity index range. It is expressed in Arabic numerals, 3. 2.2
3.2.3 Performance code indicates products of the same specification but different performance, expressed in Roman numerals. 3.2.4 The product code representation method is as follows: M
Performance code
Specification code (100)
For cellulose pith
Approved by the State Administration of Quality and Technical Supervision on September 10, 1999 For cellulose aldehyde
Implemented on April 1, 2000
4 Requirements
4.1 Appearance
GB/T91071999
Li Dingyuan Guo Gong Yuan Da Yang Zhong
The appearance of refined cotton should be uniform and loose, without any impurities such as sawdust, bamboo dust, sand, oil, metal, etc. visible to the naked eye. 4.2 Performance
The physical and chemical performance indicators of refined cotton for cellulose acetate should meet the requirements of Table 2. Table 2 Physical and chemical performance indicators of refined cotton for cellulose acetate Product model
Viscosity mPa: s
Q-cellulose content
Acid mixing degree
Upper east content
Acid insoluble matter content
Iron content
Ing/kg
Ether extract content
%Alkali soluble matter content
C100-1
71-~120
The physical and chemical performance indicators of refined cotton for nitrocellulose should meet the requirements of Table 3 C100-1
71~12 0
Table 3 Physical and chemical performance indicators of refined cotton for nitrocellulose red cellulose
α-cellulose content
Moisture content
Hygroscopicity
Ash content
Content of sulfuric acid insoluble matter
21~40%
C200-1
121~300
121~300
GB/T9107-1999
4.2.3 The physical and chemical performance indicators of refined cotton for cellulose ether shall meet the requirements of Table 4. Table 4 Physical and chemical properties of refined cotton for cellulose ether Product model mPa·s α-cellulose content Moisture content Performance index Absorption degree Ash content Sulfuric acid non-flow energy Cellulose content Absorption degree tt Absorption degree tt Iron content |121~300
If there are special requirements for the indicators, the user and the manufacturer can negotiate to determineM30
301~500
M400-1
301500
M100-1
71~120
The corresponding measured values of polymerization degree and viscosity are shown in the appendix of Appendix C), and the measurement method is in accordance with the appendix of Appendix E). 5 Test method
5.1 Sample preparation
M100-1
5b1~80o
M200-1
121~300
5.1.1 Place the received sample in a clean tray, tear it loose and mix it, but do not allow non-fiber impurities to be removed. Quickly take out the sample for measuring moisture content, and then spread out the remaining samples with a thickness of about 20mm~30mm. Place them at room temperature for 3h~4h to allow their moisture and atmospheric humidity to approach equilibrium. This sample is called a balanced sample. 5.1.2 When weighing the samples for measuring α-cellulose content, ash content, sulfuric acid insoluble content, iron content, 7.14% alkali soluble content, and copper value, weigh the sample at the same time and measure its moisture content. The measurement method shall be in accordance with the provisions of 5.3. The result is expressed to two decimal places. 3
5. 2 Determination of viscosity
5. 2. 1 Method summary
CB/T 9107 -- 1999
Use copper nitrogen solution to dissolve the sample, select a suitable capillary viscometer, and measure the time for the cellulose copper ammonia solution to flow through the upper and lower scale lines of the viscometer at a specified temperature. Calculate the viscosity of the sample. 5.2.2 Reagents and their preparation
Copper fluoride solution, in which the copper content is (1.30±0.02) g/100ml, the hydrogen content is (15.0±0.2) g/100mL, the sodium hydroxide content is 0.7 g/100mL, and the ascorbic acid content is 0.2 g/100mL. The preparation method is shown in Appendix [(Appendix of the standard). 5.2.3 Instruments and equipment
a) Constant temperature water bath heating device:
b) Glass insulation cover: see Figure 2:
c) Viscometer: see Figure 3. According to the expected viscosity of the sample, select a viscometer with different constants and capillary diameters so that the outflow time of the viscosity solution is within the range of 4U s~10 min. When performing parallel measurements in China, viscometers of the same level and with similar band numbers must be selected. Specific requirements for viscometers during the test are shown in Table 5;
d) Stopwatch: accuracy is 0.28
e) Steel ball: diameter is about 5mm-6mm
f) Vibrator;
) Copper ammonia solution injection device: see circle 4. The reagent bottle is wrapped with black cloth to avoid light: h) Viscosity measurement device: see Figure 5.
Unit: mm
#15, 5 + 1. 5
$7. 25±0.25
Figure 2 Glass insulation sleeve
Viscometer specifications
Measurement of solution viscosity
Viscometer
Constant K
Capillary inner diameter
0. 6--7.0
Table 5 Viscometer selection requirements
32-160
410= 0. 5
Figure 3 Viscometer
1110--050
160~1 200320--
1 600480-5 600
0. 01 --0. 050. 05~- 0. 150. 15 -- 0. 5c0. 50 --0. 900. 90~-1. 801. 80-- 2. 902. 90-- 5. 005. 00 ~- 7. 5c1. 0
..com4.5
GB/T9107—1999
Injection device of copper ammonia solution
Viscometer: 2-glass insulation cover: 3-funnel 4-fixed frame Figure 5 Viscosity measurement device
5.2.4 Analysis steps
5.2.4.1 Use tweezers to take samples from the dish containing the sample. The sampling points should be no less than 10. Tear and mix them evenly to remove impurities. Use a scale of known mass to weigh about 1g of the sample and place it in an oven at 105℃±2℃ to dry for 30min. Then move it into a desiccator to cool for 20min~40min. 5.2.4.2 Prepare a cellulose copper ammonia solution with a concentration of 1 g/100 mL (prepared cotton with a viscosity higher than 100 mPas at a concentration of 0.75 g/100 mL) according to the working volume of the selected viscometer. Calculate the mass of the dry sample to be weighed according to formula (1) to an accuracy of 0.005 g.
Wherein: m
m=(VV)Xc
Mass of the dry sample to be weighed, g;
Total volume of the viscometer, ml;
wm（1）
V.—Volume of the steel ball, mL:
GB/T 9107—1999
c——Concentration of cellulose copper ammonia solution.u/100 ml Note: Determination of the volume of the steel ball: At 20°C, take 1(a) steel ball of the same specification, clean and fresh, and put it into a burette filled with half-water. Calculate the average volume of each steel ball according to the number of milliliters added.
5.2.4.3 Put the weighed dry sample into the viscosity meter and add 916 steel balls (the total volume of the steel balls is 1.0 m±0.Q5 tn). Put a rubber plug with a steel ball (called a ball) at the end of the capillary of the viscometer and close it. At the neck end, plug it tightly with a rubber plug with a glass tube ball switch. Then connect the rubber hose at the end of the capillary to the lamp suction pin of the active roller. Open the piston on the iris and squeeze the ball switch on the upper and lower sides of the viscometer at the same time to make the solution flow slowly into the viscometer. Shake it several times to drive out the air. The ammonia solution should be filled to the neck. Close the ball plug and remove the viscometer. 5.2.4.4 Remove the viscometer and gently operate it several times to make the fiber case disperse. Put it in an oscillator or shake it until the sample is completely dissolved (check whether the sample is completely dissolved , and quickly observe the viscometer against the light to determine whether there is a jelly or purple substance in the viscometer). 5.2.4.5 Place the viscometer upside down in a constant temperature water bath at 20.0°C ± 1.5°C, and place it away from light for 30 minutes. 5.2.4.6 Take out the viscometer (do not let the neck face upward), wipe it, remove the rubber plug, remove the steel ball, and then plug it again. Remove the ball switch at the end of the capillary, and place a glass insulation cap at 20.0°C ± 0.5°C, and adjust it to a vertical state. 5.2.4.7 Gently pull out the cavity plug, and the solution will flow out of the capillary tube. Record the time between the upper and lower scale lines of the capillary for the cellulose copper ammonia solution to flow through the capillary, accurate to 0. 2 $，
5.2.5 Expression of analysis results
The viscosity of cellulose copper-ammonia solution is calculated according to formula (2). 7 = 0.97K
Wherein: 7--1 g/100 ml. Viscosity of cellulose copper-nitrogen solution, mPa·9; 0.97--1 g/100 ml. Density of cellulose copper-nitrogen melt line + g/cm\;K-viscometer band number
t--Time for the liquid to flow between two scale lines, s,-(2)
The viscosity of 0.75 g/100 mL cellulose copper-ammonia solution can be converted into the viscosity of 1 g/100 mL cellulose copper-ammonia solution according to formula (3). n =(7,)1-29
Wherein: n.-1g/100ml. Viscosity of cellulose copper nitrogen solution, mPa9; 7—0.75g/100mL viscosity of cellulose copper ammonia solution. mPa*s; Two results are measured in parallel for each sample, and the relative allowable difference does not exceed 10%. Take the arithmetic mean and express it to the integer. 5.3 Determination of water content
5.3.1 Summary of the method
After drying the sample, measure its weight loss; calculate the moisture content of the sample. 5.3.2 Instruments and equipment
) Weighing blood;
b) Oven:
c) Drying.
5.3.3 Analysis steps
Use a dry scale of known mass to weigh 3 to 5 grams of the sample before equilibrium, accurate to 0.001 g, put it in an oven, dry it at 105°C ± 2°C for 6 hours, or dry it at 135°C ± 2°C for 30 minutes (infrared or other verified drying methods are allowed). Take out the scale, cover it, and quickly move it into a desiccator. After cooling for 30 minutes to 60 minutes, weigh it to an accuracy of 0.001 g. 5.3.4 Expression of analysis results
The moisture content in the sample is calculated according to formula (4):
ml -m2 × 100
W(4
武中：
GB/T 9107—1999
- Mass fraction of water in the sample, %;Www.bzxZ.net
- Mass of blood and sample before drying·m. Mass of blood and sample after drying·g+m-mass of sample+g.
Two results are measured in parallel for each sample, and the difference is allowed to be no more than 0.5%. Take the arithmetic mean. The result is expressed to one decimal place. 5.4 Determination of α-cellulose content
5.4.1 Summary of the method
Use a cellulose with a mass fraction of 17.5% After the sample is treated with sodium hydroxide solution: filter, wash to neutral, dry, weigh, and then calculate the amount of residue (α-cellulose).
5.42 Reagents and their preparation
a) Glacial acetic acid: GB/T676, prepare a 10% volume fraction drop; b) Sodium hydroxide solution: first use solid sodium hydroxide (GB209) and add water to make a 50% mass fraction solution, put it in a closed bottle, cover it for more than 1.5 days, so that the carbonate is fully precipitated until the solution is clear. Use a siphon to absorb the upper clear solution, and then use distilled water without carbon dioxide to prepare a solution with a mass fraction of 17.4%~17.6%, and the mass fraction of carbon dioxide is not more than 0.3%. 5.4.3 Instruments and equipment
a) Porcelain cup: 250mL500mlL;
b>Filter cup: filter plate aperture is 20m~40m
c Suction flask: 1000mL~1500mL
d) Water flow pump or vacuum pump,
e) Volumetric flask: 50mL~100mL;
1 Thermometer: 0C~50℃. Graduation value is 175C; g) Constant temperature water bath installation device.
5.4.4 Analysis steps
Place the porcelain cup containing 30mL sodium hydroxide solution [5, 4.2b]] and the bottle containing distilled water without oxidation in a constant temperature water bath at 20.0±0.5℃ and keep warm for 10min. 5.4.42 Weigh about 2g of the balanced sample, accurate to 0.0002g, and place it in a porcelain cup. Stir carefully with a flat glass rod and flatten the sample. Cover the surface with blood and place it for 30 minutes. Stir it occasionally for about 1 minute each time. Then add 30mL of hot water without carbon dioxide and continue stirring for 1 minute to make it a uniform paste. 5.4.4.3 Filter it under reduced pressure with a filter cup of known quality, absorb the alkali solution, and then wash it with 700mL of distilled water several times. 5.4.4.4 Remove the filter cup, add 30mL of glacial acetic acid solution [.5.4.2a)], soak for 5 minutes, filter it under full pressure, and wash it with hot distilled water to neutralize it (check with lycium paper). After absorbing it, remove the filter cup and put it in an oven. Keep it at 135°C ± 2°C for -1 sec. 5.4.5 Expression of analysis results
The content of α-cellulose in the sample is calculated according to formula (5): mm
= m×(1 =5 × 100
Wherein, w is the mass fraction of a-cellulose in the sample, %, m is the mass of the filter residue and filter cup after drying, g; m3 is the mass of the filter cup, g1
mu is the mass of the equilibrium sample, multi
is the mass fraction of water in the equilibrium sample, %. Two results are measured in parallel for each sample, and the difference is allowed to be no more than 0.3%. The arithmetic mean is taken and the result is expressed to the decimal place. 5.5 Determination of moisture absorption
5.5.1 Method Abstract
GB/T9107
Immerse the sample in water at a specified temperature and keep it for a certain period of time, then weigh the sample after absorbing water and calculate the moisture absorption of the sample. 5.5.2 Instruments and equipment
a) Special aluminum cylinder: see Figure 6, with aluminum pan; b) Thermometer: 0c~50c, graduation value is 1c; c) Water container: about 120mm high, diameter or side length is about 160mm; d) Industrial balance;
e) Stopwatch.
5.5.3 Analysis steps
Weigh about 15g of the balanced sample, accurate to 0.1g, and evenly place it in a special aluminum cylinder of known mass. Use an aluminum plate to press the sample accurately to the 50mm mark inside the cylinder, and then steadily immerse it in a container filled with 20.C ± 2.C distilled water (the water volume in the container must not be less than two-thirds of its height) to the 8mm mark outside the cylinder. After leaving it for 30s, quickly take it out and place it in an aluminum pan and weigh it, accurate to 0.5g. 5.5.4 Expression of analysis results
The humidity absorption of the sample is expressed according to the formula
(6)
Where: m
Humidity absorption of sample
Mass of the sample and aluminum cylinder (including aluminum pan) after absorption gMass of the aluminum cylinder (including aluminum pan), g
Mass of the balanced sample·g.
Each sample
Two results are measured, and the relative allowable difference does not exceed 5%. The arithmetic mean is taken and the result is expressed to the integer.
5.6 Determination of ash content
5.6.1 Summary of method
Figure 6 Aluminum tube for measuring moisture absorption
Unit: mm
Number of holes 29
Number of holes 14
GB/T9107
Carbonize the sample, burn it in a high-temperature furnace, cool it, weigh it, and calculate the ash content of the sample. 5.6.2 Instruments and equipment
a) Porcelain: 50ml~100ml;
b) High-temperature furnace;
c) Dryer.
5.6.3 Analysis steps
Weigh about 5g of balanced sample, accurate to 0.01g, place in a container of known mass, half-cover, and slowly carbonize on an electric furnace (avoid coloring). After carbonization, burn in a high-temperature furnace at
for 1h, take out, place in the air for 5min, move to a desiccator and cool for 30min~60min, and weigh to a constant weight. Accurate to 0.0002g. 5.6.4
Expression of analysis results
The ash content in the sample is calculated according to the formula (
Wherein: w3
Mass fraction of ash in the sample
Mass of slag after ignition and
Mass of the balanced sample-g:
Mass fraction of water in the balanced sample
The average value of each sample, the result table
5.7 Determination of sulfuric acid insoluble matter
Method Summary
# Two decimal places are allowed.
(7)
10.03%)), take the calculated value
After dissolving the sample with cold concentrated sulfuric acid, add water to dilute, filter, wash, dry and weigh, calculate the sulfuric acid insoluble matter content of the sample. Formula and its preparation
Instruments and equipment
Porcelain cup: 250m
b) Filter cup: filter plate hole spring
c) Measuring cylinder: 50mL;
Beaker: 800
Filter bottle: 1000mL
) Water flow pump or vacuum pump;
) Flat-headed glass rod: the diameter of the flat head is about romm. 5.7.4 Analysis steps
Weigh about 10g of the balanced sample, accurate to 0.01g. Place the dry porcelain cup in cold water with a temperature not exceeding 20C, and inject 35mL~50mL of sulfuric acid cooled by water below 15C, then add the sample several times and stir quickly to dissolve the sample completely until it becomes a uniform colloid (about 5min~10min, if white blocks appear, use a flat-headed glass rod to grind for 2min~3min to dissolve it as much as possible). Then take the porcelain cup out of the cold water, wipe the outer wall dry, and slowly pour the contents of the porcelain cup into a beaker containing 400mL-500mL distilled water while stirring. All the residues attached to the wall of the porcelain cup should be washed into the beaker, diluted with water to about 800mL, and allowed to stand until the residue settles. Then, filter it with a dry filter cup of known mass under a slight reduced pressure, and wash it with hot water until it is neutral. Remove the filter cup, wipe the outer wall dry, place it in an oven at 135C ± 2℃ and dry it for 30 minutes, transfer it to a dryer and cool it for 30 minutes to 60 minutes, and weigh it to a constant weight, accurate to 0.0002g. 5.7.5 Expression of analysis results
The content of sulfuric acid insoluble matter in the sample is calculated according to formula (8). 903%), take the calculated
After dissolving the sample with cold concentrated sulfuric acid, add water to dilute, filter, wash, dry and weigh, calculate the sulfuric acid insoluble content of the sample. Reagent and its preparation
Instruments and equipment
Porcelain cup: 250m
b) Filter cup: filter plate hole spring
c) Measuring cylinder: 50mL;
Beaker: 800
Suction flask: 1000mL
) Water pump or vacuum pump;
) Flat-head glass rod: the diameter of the flat head is about romm. 5.7.4 Analysis steps
Weigh about 10g of the balanced sample, accurate to 0.01g. Place the dry porcelain cup in cold water with a temperature not exceeding 20°C, and add 35mL~50mL of sulfuric acid cooled by water below 15°C. Then add the sample several times and stir quickly to dissolve the sample completely until it becomes a uniform colloid (about 5min~10min. If white blocks appear, grind them with a flat-headed glass rod for 2min~3min to dissolve them as much as possible). Then take the porcelain cup out of the cold water, wipe the outer wall dry, and slowly pour the contents of the porcelain cup into a beaker containing 400mL500mL of distilled water while stirring. All the residues attached to the wall of the porcelain cup should be washed into the beaker, diluted with water to about 800mL, and allowed to stand until the residue settles. Then use a dry filter cup of known mass to filter under slight reduced pressure, and wash with hot water until neutral. Remove the filter cup, wipe the outer wall dry, place it in an oven at 135°C±2°C for 30min, move it to a desiccator to cool for 30min~60min, and weigh it to a constant weight with an accuracy of 0.0002g. 5.7.5 Expression of analysis results
The content of sulfuric acid insoluble matter in the sample is calculated according to formula (8).03%), take the calculated
After dissolving the sample with cold concentrated sulfuric acid, add water to dilute, filter, wash, dry and weigh, calculate the sulfuric acid insoluble content of the sample. Reagent and its preparation
Instruments and equipment
Porcelain cup: 250m
b) Filter cup: filter plate hole spring
c) Measuring cylinder: 50mL;
Beaker: 800
Suction flask: 1000mL
) Water pump or vacuum pump;
) Flat-head glass rod: the diameter of the flat head is about romm. 5.7.4 Analysis steps
Weigh about 10g of the balanced sample, accurate to 0.01g. Place the dry porcelain cup in cold water with a temperature not exceeding 20°C, and add 35mL~50mL of sulfuric acid cooled by water below 15°C. Then add the sample several times and stir quickly to dissolve the sample completely until it becomes a uniform colloid (about 5min~10min. If white blocks appear, grind them with a flat-headed glass rod for 2min~3min to dissolve them as much as possible). Then take the porcelain cup out of the cold water, wipe the outer wall dry, and slowly pour the contents of the porcelain cup into a beaker containing 400mL500mL of distilled water while stirring. All the residues attached to the wall of the porcelain cup should be washed into the beaker, diluted with water to about 800mL, and allowed to stand until the residue settles. Then use a dry filter cup of known mass to filter under slight reduced pressure, and wash with hot water until neutral. Remove the filter cup, wipe the outer wall dry, place it in an oven at 135°C±2°C for 30min, move it to a desiccator to cool for 30min~60min, and weigh it to a constant weight with an accuracy of 0.0002g. 5.7.5 Expression of analysis results
The content of sulfuric acid insoluble matter in the sample is calculated according to formula (8).
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