Some standard content:
ICS 71. 060. 2G
National Standard of the People's Republic of China
CB/T19591—2004
Issued on September 29, 2004
Titanium dioxide
Nano-titaniur dinxidc
Implemented on April 1, 2005
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China Standardization Administration of China
This standard is formulated according to the standards of nano-titaniur dinxidc manufacturers and actual product data within the period. This standard is issued by the Ministry of Science and Technology of China. This standard is issued by the Shandong Provincial Chemical Standardization Committee (SAC/Te2/SCI1). The sponsor of this standard is China Guangyang Chemical Research Institute, GB/T19591--2004. The sponsors of this standard are: Jinan Gexing Chemical General Factory, Jiangsu Huihai Nanotechnology Co., Ltd., Shenzhen Chengshi Technology Co., Ltd., Ganruimeidi Nanomaterials 71 Development Co., Ltd. Sichuan: The drafters of the standard are Yao Minggui, Dui Anruo, Qu Meigan, Xing Jinsong, Xue Weiguo, and Youjiu Zhengyueying. T
1Fan Guo
Nano titanium dioxide
CB/T19591-2C04
This standard specifies the oxygen content, requirements, test methods, inspection rules, marking and labeling, packaging, transportation and treatment of rice "oxygen ratio". This standard applies to nano titanium dioxide beverages. The main use of this product is Ding Fangming cosmetic value, kinetic energy Chemical fiber, high-grade plastic, paint, oil device, coating, electronic system, chemical testing technology and its carrier and other fields. Molecular formula: TiO
Molecular weight: 79.8: 201 International Relative Quality) 2 Normative reference documents
The clauses in the following documents are regarded as clauses of this standard through reference in this standard. For all the referenced documents with different dates, all the subsequent revisions (excluding the contents of the station) or revised versions are not applicable to this standard. This standard. However, it is encouraged that if the latest version of the relevant document is used according to the relevant agreement of the wood standard, the latest version of the referenced document shall be used for the wood standard. R/T1912000 Package end transport element standard
GR/T1250 Limit value method and delimitation method GH/T2922 Chemical test method for specific surface area of color carrier 1986 General rules for sampling of chemical products
G/T Sa
【/5532—1992 Laboratory water temperature and test methods (ncIS369F: 1987] Chemical products sanitary chemical standard test method G/117
GB/17917.2—1987 Chemical products sanitary chemical standard test method B/T79:7.31987 Cosmetics 1 Core chemical standard test method H/T3G96.1 Preparation of standard titration solutions for chemical analysis of inorganic chemical products H/T36%.2 Light Preparation of standard solutions for chemical analysis of organic chemicals Preparation of preparations and products for chemical analysis of inorganic chemicals HG:T36$6.H
3 Product classification
The types of titanium dioxide can be divided into two types: nano-titanium dioxide (A1) and nano-titanium dioxide (R), which are respectively expressed as nmT:O,(A).mwTiO,(R)
4 Requirements
4.1 Appearance: Color powder.
4.2 Nano-titanium dioxide should meet the requirements of Table 1 CB/T [9591—2004
The amount of the chemical or chemical number of the total effect 6
Single slow in the approximately necessary diameter/
R1>Around the chemical average particle size/Tm
Ratio table product/m/
Group index
To (Hg) section differential
F (A's opening fraction
Assumed mass common number
Yonghao's mass single fraction/y
White sea/wine
11 In the blood to appear oxidation deficiency, the single opening standard of 10% can be set as the will, so that the two must be in danger for the body energy quality, 2) for the chemical product, the medical more slowly increase the control safety indicators: test method
5.1 Safety data
Some of the reagents used in this test method are toxic or corrosive. Be careful when operating! If it comes into contact with the skin, flush it with water immediately and seek medical treatment immediately. When using disposable products, it is strictly forbidden to use eyeglasses to heat them. 5.2 General provisions
The reagents used in this standard shall be the first-class water specified in G/T66$21992 when the type of the water bath is specified, the standard titration solution, the preparation and the product in the test shall be the standard HG/TESE specified system when the type of the water bath is specified.
5.3 Determination of product type
5.3.1 Receiver
5.3.1.1 X-ray diffraction test,
5.3.1.1 X-ray diffraction test,
5.3.1.1 X-ray diffraction test, power: 43kV/um.A. 5.3.2 Analysis Steps
Place the sample in the diffraction analyzer according to the requirements and then enter the diffraction analyzer for determination. Adjust the instrument to allow the sample to be measured and the height of the diffraction analyzer to be within the range of 20 to 30 degrees. (The main surface of the sample with rutile type 10 is sharp and the sample has a main surface with 10 degrees of cut.) 5.4 Determination of Titanium Dioxide Content
5.4.1 Method summary
Use concentrated sulphuric acid and energy to dissolve the sample, and use the atmosphere of carbon monoxide to reduce aluminum to titanium (and). The reducing solution is titrated with standard acid or acid as indicator. 5.4.2 Reagents
5.4.7.1 Sulphuric acid:
5.4.2.2 Monitor:
5.4.2.3 Gold foil: mass fraction not less than UJ, >%, thickness 0.1mm: 5.4.2.4 Ammonium sulfate;
5.4.2.5 Magnetic acid hydrogen saturation evaluation solution:
5.4, 2. Iron is eliminated by standard galvanic wave [NH4+Fe(S)]. About 0, mal/L; GB/T:19591-2004
Take lead ammonium [NTI,Fe(S,::] and place it at 10 00m. Volume, Sichuan people contain m aviation acid mL drop part, simple cIKMn=3,: mnl/I high-tech gland clock report, straight year drop 7 net red door water weighing release to the scale and if the box policy does not eliminate, then filter, use the oral dioxide method to certify the substance, 1, 1 now determine the extraction step is to carry out the standard.
The standard ammonium hydroxide solution is full of this concentration [>El, Fe(St), the accurate value, the unit is liter and then rsoi/) formula (1) bucket concentration:
The titration energy consumption is the value of the standard titration flow, you are Tongli (): Yi--
L—standard substance P1<, the value of mass efficiency (using the spectrum ton 1i). 1H to calculate?: The value of the standard drug production mass, the unit is gram you rate (g/101 before = 79.33)
The number of the standard substance of dioxide, the unit is point () 5.4.2.7 Vegetable zero ammonium indicator. 215 g/. Melting slope: 5.4.3 Receivers and equipment
5. 4.3. 1 Oven; can select the temperature of 1 (;--=3 yuan 5.4.3.2 or other suitable absorption income! 5.4.3.3 Electric heating constant benefit dry frequency alliance, the inner package also has 1 drying model, such as silicon collection. 5.4.4 Analysis steps
Weigh the pre-light in (35--110)\ stained 2 test + (0.19--0.21)g fine to G.603! -)
Add acid to the sample in the U chain travel. Make sure that the acid is fully reported, and heat slowly: heat again until the test column will shrink to form a drop liquid, cool and add. Water and plate acid, spoon Add 2 more gold flakes, fill the liquid, add hydrogen peroxide and solution to the tube until it is about 2/3 of the volume. When the aluminum flakes are completely added, the solution will boil slightly: 3-31min. At this time, the solution will be transparent and will not stop secreting. In this process, sodium bicarbonate and solution should be added at any time. Do not let it absorb air. After cooling, remove the liquid on the conical collection bottle and put the saturated solution of magnetic acid in the tube into a low-profile bottle. Quickly adjust the titration with ferrous sulfate solution. When it is close to the end point, add 2mL of ferric acid before the end point indicator. Continue to titrate until it is light. 5. 4. 5 Results
Annual content is calculated as carbon dioxide! The mass fraction is expressed in % and is calculated as follows: h-ms × 100 - G1M
The value of the internal position of the titration of the ammonium hydroxide standard (..4.2.) is expressed in millimeters (mT). The standard liquid is closely connected to the standard value of the sample mass (in grams):
The integral value of the mass fraction of the oxide is expressed in grams (/m5=79.88): Note: Before the product is calibrated, the company must take the average value of the parallel measurement results as the target value. The absolute difference between the two parallel measurement stations shall not be less than 5.5. Determination of the average particle size under electron microscope. Take titanium dioxide sample and use 1-1% ethyl acetate as the reagent. After reading the ultrasonic data, collect (1-2) drops of noise at intervals. Place it on the sample stage of the electron microscope and magnify it by about 110,000. Select the particles with obvious differences in the area and take a fast electron microscope picture. Use a nanometer ruler to measure the length and width of each particle in the photo (computer software can be used for statistical processing):, take the arithmetic mean, and calculate the average particle size according to the formula:
=2(d.+d.)
(+d,)-the sum of the diameters of the micrometer ruler, the unit is nanometer (m); measure the total length of each particle:
5.6 Determination of average particle size by XRD line broadening method 5.6.1 Reagents
5.6.1.1 Customer silicon standard sample.
5. 6.2 Instruments
5.6.2.1X and/or diffraction detector;
5.6.2.1.1X time-domain transmitter, 40kV/30mA, 5.6.3 Analysis steps
Set the sample to X-ray diffraction measurement after sample preparation, adjust the X-ray diffraction peak height of the sample to within the recorded range, adjust the instrument with the same method as the sample, and determine the The characteristics of the surface: take the 8.4 half-width of the polysilicon as the reference half-width, measure the peak width of the sample surface, and calculate the average surface area using the Scherrer formula.
27 degrees for the golden red crystal, the angle is from 2:
sharp point 101 degrees for the crystal 25 degrees: the angle range is from 23\-~27°5.7 Determination of specific surface area
called the European test column, call to 1.1. Find H/2922 Heat solid measurement. It can also be measured using the standard sample provided by the instrument.
5.8 Determination of agglomeration index
Take about 0.01% of the oxidized test particles, add (2-3) sodium dodecyl benzoate solution to the mixture, and use a glass to gradually separate them. Then add 20 ml of water and use a super-high power of C to separate them. The average particle size of the sample can be measured according to the sampling requirements of the mass spectrometer (maximum 92 μm-10). D The half-average particle size obtained in 5.6 is used as the average diameter of the primary particles.
Agglomeration index () is calculated as follows:
In the calculation:
1 minute, the average value of the agglomerate particles is obtained by the micro-light particle analyzer, in nanometers. Calculate (): =, the average particle size of the secondary particles obtained in 6 steps, in nanometers (r). 5.9 Determination of mercury content
Calculate the content according to H, 17917.-237, 5. \Q Determination of content
The content of lead shall be determined in accordance with the provisions of GB/T 517.2-187. 5.11 Determination of lead content
The content of lead shall be determined in accordance with GB/T 517.2-187. 5.12 Determination of moisture
5.12.1 Method
Under certain pressure conditions, the sample is weighed down to a constant weight, and the weight is determined based on the reduced mass of the sample. 5.12.2 Instrument
5.12.2.1 Weighing bottle: 50mm×25mm
5.12.2.2 Electric heating constant group upper refining box: Salt Huineng fall made in (105~110>T:.GB/T 19591--2004
5.12.3 Analysis steps
Use a constant-weight flask that has been exposed to light at (195-110℃) to weigh about 1g of the sample (to be determined by weighing to 1g). Place it in an oven and wait for (105--11) hours until the sample is weighed.
5.12.4 Calculation of results
The moisture content before drying is expressed as % and is calculated according to formula (5): = × 100
In the process:
The value of the mass of the flask and the sample before drying is in grams (); the number of the sample weighed after operation is in grams (); the value of the sample pressure gain is estimated in grams (in grams). n
Take the average value of the elasticity of the half-row determination as the solid result, and the pre-modification of the half-row determination result is not much. 2. 5.13 Determination of pH value
5.13.1 Reagents
5.13.1.1 Do not contain water monoxide.
5.13.2 ApparatusWww.bzxZ.net
5.13.2.1 The range of the pH value is -100025. 13.2.2 Reference electrode; 5.13.2.3 Ice electrode, centrifugal break:
5.13.2.4 Repeat.
5.13.3 Analysis steps
Connect the reference string and the measuring electrode to the stability meter and adjust the position. Weigh (1).1=0.01> sample, put it in a 150mL beaker, add 16gmT of carbon dioxide, mix well, set the value of 3)ir with acid ecological solution, take the arithmetic mean of the parallel determination results as the determination result, the absolute difference of the two half-determination results shall not be greater than CRpTI5.14 Determination of whiteness
5.14. 1 Rapid instrument
5. 14. 1. Whiteness or color determination
shall meet the following requirements:
: The full wavelength is generally (38m-72>m and cannot be less than (400750)m. The half-width of the wavelength: the half-width of the wavelength emitted by the photometer is more than 1nm. c) The optical accuracy should be within U.5% of the optical range: the deviation between the nominal concentration and the actual instrument return value shall not exceed).5nm. 5.14.1.2 Mixing and mixing
5.14.2 Analysis
5.14.2.1 Sampling
Take a certain amount of sample and put it into the instrument. Make the sample plate flat, ineffective, and without any spots. Each batch of products needs to be made into: 100 sample plates
CR/T 19591—2004
5.14.2.2 Calibration of the instrument
Use the standard plate to calibrate 1. Start with the standard plate, warm up the instrument according to the instructions, and adjust the zero value. Use the working plate to calibrate the instrument
5. 14. 2. 3 Measurement
Put the fast sample plate on the test bench or measure the value of each sample plate. Take a sample plate and measure the average value of the results: 5.14.3 Calculation of results
5.14.3.1 Calculation of the chromaticity coordinates of the sample. -X..(X.+Y...-Z..)
y..-Y....x. -- Y.....
ay=Z(Xn
5,14.3.2 Calculation of the chromaticity
Calculate the difference between the chromaticity () and the chromaticity () according to the common or ():
BY: +400 -30003: +235.
.YZ.-…are the values of the standard field sensitivity of 10 respectively; the standard color is pure.
Take half of the result of the calculation as the standard result, and the absolute difference between the results of the single determination shall not exceed 3.5. 5.5 Determination of bulk density
5.:5.1 Method
A certain amount of sample is passed through a cone hopper and placed in a circular material passage of a known volume, and the amount of the sample filled is determined. 5.15.2 Approximately
5.15.2.1 Determination of bulk density The apparatus for determining bulk density is shown in Figure 1. The apparatus for determining bulk density
5.15.2.2 Material determination:
Put the material on a plate, a glass plate, a weighing ball and a blasting plate as the measuring device. 1R, carefully add water to the filter, when it is almost full, add water with a dropper, [. Glue the filter, use a filter to absorb the water on the outside of the filter and the filter, and there should be air bubbles between the filter and the water. Then weigh the mass of the filter and the filter, the viscosity is 0.1R, the volume of the filter, and the value is expressed in grams (g). The following are the calculation results: 5
In the calculation:
The value of the amount of water in the filter and the filter, the unit is gram (g); the value of the particle size of the final water and the air volume of the segment, each unit is gram (g); **
The value of the pure water is calculated at the time of
, the unit is gram/liter (g/mL); the filter volume is calibrated at least once a month. 5.15.3 Analysis step
Install the stacking determination device according to Figure 1, take the material base, and the accuracy is more than 1.
GJI/T10591—2004
Close the bottom of the bucket. Put the sample on the side naturally, scrape off the high white part with a knife and put it back into the material with known quality. Then open the bottom of the bucket to make the test sample flow into the beach automatically. Remove the high part on the ruler (do not move the end of the sample before brushing it flat). Weigh the quality of the test sample and the sample, accurate to 1 s.
5.15.4 Calculation of the density The density is expressed in grams per litre/ml.) Formula 8) Calculate the mass of the material p = m2 - the mass of the material in grams (s) - the volume of the material in milliliters (ml). Take the arithmetic half of the results of the parallel determination as the test result. The difference between the two parallel determination results shall not exceed (.2g/mL): 6 Inspection rules 6.1 This standard applies to type inspection and factory inspection. 6.1.1 All twelve indicators in the requirements are type inspection items. Under normal production conditions, type inspection shall be carried out every six months. 6.1.2 The heat content, moisture content and pH value of the table must be inspected before delivery. 6.2 Take one batch of products produced per day as one batch. 6.3 According to (T557- 6.3 The number of sampling units shall be determined as per the provisions of Article 19. When sampling, the sample shall be placed vertically in the sampler until the sample is 3/1 of the depth of the material layer. The sampled products shall be mixed and divided into two clean and wide-mouthed plastic bags and sealed. Note the manufacturer name, product name, type, batch number, sampling date and sample name: one copy shall be used for inspection, and the other shall be kept as a backup set. The storage time shall be determined based on the actual collection conditions. 6.4 The production plant's pressure supervision and inspection department shall inspect and accept the nano titanium dioxide in accordance with the provisions of this standard. The production plant shall ensure that each batch of products leaving the factory meets the requirements of this standard. 6.5 The user unit has the right to inspect and accept the nano titanium dioxide received in accordance with the provisions of this standard. The inspection shall be carried out within 1 month from the date of receipt. ||6.6 If any of the indicators do not meet the requirements of this standard, retest the samples from the packaging. If the test results do not meet the requirements of this standard, the whole batch of products shall be deemed unqualified. 6.7 If the test results do not meet the requirements of this standard, the specified values specified in CB/T1251 shall be used as much as possible. 7 Marking and labeling
7. The brand name of calcium dioxide shall be marked with the manufacturer’s name, factory name, product name, category, batch number or production phase and this standard number, as well as the “Nanjing Mark” specified by GW/TIS12000 B19591--2004
7.2 Each batch of nanometer dioxide shall be accompanied by a quality certificate, including: manufacturer’s name, product name, category, trademark, etc. Content, batch number or production date of the product, quantity and compliance with this standard shall be proved by the market standard. 8. Packaging, transportation and storage || tt || 8.1 The packaging of nanometer dioxide materials shall prevent the product from being squeezed and re-aggregated. The outer packaging shall be flat paper barrel or plastic barrel packaging. The inner packaging shall be made of two layers of polyurethane film. The inner bags shall be tied with pure or other materials of equivalent quality, or other types of bags. The net content of each bag shall be 5kg and 15kg. Or the packaging method and specifications shall be negotiated with the user. 8.2 During the transportation process, nanometer dioxide sensitive substances shall be carefully selected. Avoid rain, smoke, and other hazards. The transportation process shall be carried out in a safe manner. The following procedures shall be followed: 1. Use containers or racks as much as possible. Transportation shall not be carried out in accordance with the standard. 2.3 Nanometer dioxide materials shall be stored in a cool and dry place away from rain, smoke, and other hazards. Avoid mixing with similar items.
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