Some standard content:
National Standard of the People's Republic of China
Titanium dioxide pigments
Titanium dioxide pigments
This standard refers to the international standard ISO591--1977 "Titanium dioxide pigments for paints". 1 Subject content and scope of application
GB1706--93
Replaces GB1706-88
This standard specifies the technical requirements, test methods, inspection rules, marking, and packaging of titanium dioxide pigments , Transportation and Storage This standard applies to titanium dioxide pigments produced by sulfuric acid or chloride methods. Products are mainly used in coatings, inks, rubber, plastics and paper industries.
Molecular formula: TiO2.
Relative molecular mass: 79.88 (1987 International Relative Atomic Mass) 2 reference standards
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB601.
GB1250||tt ||Expression method and judgment method of limit values ??GB1717
GB1864
Determination of pH value of pigment aqueous suspension
Comparison of pigment colors
Basic environmental testing of electrical and electronic products Regulations Guidelines for Damp Heat Test GB2424.2E
GB5211.2
GB5211.3
GB5211.12
GB5211.14
GB5211.15|| tt||Determination of pigment water-soluble content Thermal extraction method
Determination of pigment volatiles at 105°C
Determination of resistivity of pigment aqueous extract
Determination of pigment sieve residue mechanical flushing method
Determination of pigment oil absorption
GB5211.16
GB6682
GB9285
3 product classifications
Comparison of the achromatic power of white pigments
Analytical laboratory water specifications and test methods Sampling of raw materials for paints and varnishes
According to the crystal form of the pigment, titanium dioxide pigments are divided into two categories: anatase type and rutile type, and each type is divided into the following Breeds and grades. Anatase titanium dioxide BA01-01 is superior product, first-class product and qualified product. Anatase titanium dioxide BA01-02 is an excellent product, a first-class product and a qualified product. Rutile titanium dioxide BA01-03 is superior product, first-class product and qualified product. The State Bureau of Technical Supervision approved the implementation on 1994-10-01 on 1993-12-30
4 Technical Requirements
GB1706-93
Titanium dioxide pigments should comply with the technical requirements listed in the table below. Item
Item
TiO content, % (m/m)
Color (compared to standard sample)
Achromatic power (compared to standard sample)||tt ||105℃ Volatile matter, % (m/m)
>
After pretreatment at 23±2℃ and relative humidity (50±
5)% for 24 hours, 105℃ Volatile
substances, % (m/m)
water-soluble substances, % (m/m)
pH value of aqueous suspension
oil absorption, g/100g| |tt||Screen residue (45μm mesh), % (m/m) water extract resistivity, Qm
BA01—01
Superior product
Approximate||tt ||100
0.4
6.5~
8.0
22
0.05
30
First-class product|| tt||Qualified product
98.0
not less than
100
0.5
0.5www.bzxz.net
0.5
6.5~
8.0
26
0.10
20
is slightly different from
90
0.6
6.0 ~
8.5
28
0.30
16
refers to
standard
BA01-02
Premium product
Approximate
100
0.3
6.5~
8.0
22
0.05
100
Equal products
92.0
Not less than
100
0.8
0.8
0.3||tt| |6.5~
8.0
26
0.10
50
Note: The standard sample of the superior product is the selected similar product; the first-class product and the qualified product The standard sample is the same sample used for selection. 5 Test method
Qualified product
slightly different from
.90
0.5
6.0~
8.5
28
0.30
50
BA01—03
Premium product
Approximate
100
0.3
6.5~
8.0
20
0.05
100
All reagents should be analytical grade reagents, and use the third-grade water specified in GB6682 or the corresponding purity of water. 5.1 Determination of titanium dioxide content
There are two methods: Method A (metal aluminum reduction method) or Method B (zinc amalgam method), both of which can be used for routine analysis and arbitration. 5.1.1A method metal aluminum reduction method
5.1.1.1 Principle
Equal products
90.0
Not less than
100
1.0
1.5
0.3
6.5~
8.0
23
0.10
50
Qualified product
is slightly different from
90
0.5
6.0~
8.5
26
0.30
50
The sample is dissolved in concentrated sulfuric acid and ammonium sulfate. Titanium (V) is reduced to titanium (I) using metallic aluminum in a carbon dioxide atmosphere. The reduced solution was titrated with ammonium thiocyanate as indicator and ferric ammonium sulfate standard titration solution. 5.1.1.2 Reagent
5.1.1.2.1 Metal aluminum sheet: content is not less than 99.5%, thickness is 0.1mm. 5.1.1.2.2 Ammonium sulfate (GB1396).
5.1.1.2.3 Ammonium thiocyanate indicator (GB660): 245g/L solution. GB1706-93
5.1.1.2.4 Ferric ammonium sulfate standard titration solution: c[NH,Fe(SO),]=0.06mol/L. Weigh 30g of ferric ammonium sulfate [NH,Fe(SO,)·12HzO) and place it in a 1000mL volumetric flask. Add 30mL of potassium permanganate solution containing 30mL of sulfuric acid (-KMnO,) = 0.1mol/L until the solution turns pink. , dissolve with 300mL of water from (5.1.1.2.7). Add c water dropwise to dilute to volume and shake well. If the solution is unclear, filter it and use 0.19~0.21g titanium dioxide standard reference material for calibration according to the operating steps specified in 5.1.1.4.
The concentration of ferric ammonium sulfate standard titration solution is calculated according to formula (1): c(NH,Fe(SO,),] =0. 079 9XV,
p·mi
In the formula: c(NH,Fe(SO,),)——concentration of iron ammonium sulfate standard titration solution, mol/Lmi-
mass of titanium dioxide standard reference material, g; V,——titration consumption of sulfuric acid The volume of ferric ammonium sulfate standard titration solution, mLp - TiO2 content in the standard reference material (if spectrally pure TiOz is used, p is calculated as 100%) (1)
0.0799 and 1.00mL ferric ammonium sulfate standard titration solution (c[NH,Fe(SO,),)=1.000mol/L) is equivalent to the mass of titanium dioxide expressed in grams. 5.1.1.2.5 Hydrochloric acid (GB622): p1.18g/mL. 5.1.1.2.6 Sodium bicarbonate (GB640) saturated solution. 5.1.1.2.7 Sulfuric acid (GB625): p1.84g/mL. 5.1.1.3 Instruments
5.1.1.3.1 Balance: sensitivity 0.0001g. 5.1.1.3.2 Oven: capable of maintaining a temperature of 105 to 110°C. 5.1.1.3.3. Glass liquid-sealed tube: See Figure 1. or other suitable absorber. 5.1.1.3.4 Desiccant: Contains suitable desiccant, such as silica gel. Figure 1 Glass liquid sealed tube
5.1.1.4 Operation steps
5.1.1.4.1 Sample
Weigh 0.19~0.21g of the sample that has been dried at 105~110℃ for 2 hours , accurate to 0.000.1g. 5.1.1.4.2 Determination
Place the sample in a 500mL Erlenmeyer flask, add 10g ammonium sulfate (5.1.1.2.2), 20mL sulfuric acid (5.1.1.2.7) and shake well. Start heating slowly, and then heat strongly until the sample is completely dissolved into a clear solution. After cooling, add 50mL water and 25mL hydrochloric acid (5.1.1.2.5), shake well, and add 2.5g of metal aluminum flakes (5.1.1.2.1). Install the liquid-sealed tube, plug the rubber stopper tightly, and add saturated sodium bicarbonate solution (5.1.1.2.6) to the tube to about 2/3 of the tube volume. After the aluminum flakes are completely dissolved, continue to boil slightly for 3 to 5 minutes. At this time, the solution turns into a transparent and clear purple color. Cool to room temperature in running water. During this process, saturated sodium bicarbonate solution should be added at any time (be careful not to allow it to inhale air). After cooling, remove the liquid seal tube on the Erlenmeyer flask, pour the saturated sodium bicarbonate solution into the Erlenmeyer flask, quickly titrate with ferric ammonium sulfate standard titration solution (5.1.1.2.4), and add sulfur when near the end point. 2 mL of ammonium cyanate indicator (5.1.1.2.3), continue titration until light orange. 5.1.1.5 Expression of results
GB1706-93
TiO2 content, expressed as mass percentage, calculated according to formula (2): 0.0799Xc·V
TiO,% =||tt ||m2
In the formula: cThe actual concentration of the ferric ammonium sulfate standard titration solution, mol/L; V,—the volume of the ferric ammonium sulfate standard titration solution consumed by the titration, mL: m—the mass of the sample, g ;
100
(2)
0.0799 - equivalent to 1.00mL ferric ammonium sulfate standard titration solution (c[NH,Fe(SO,))=1.000mol/L) The mass of titanium dioxide expressed in grams.
Note: The difference between the room temperature when the ferric ammonium sulfate standard titration solution is calibrated and the room temperature when used should be within 5°C, otherwise it will need to be recalibrated. 5.1.2B method zinc amalgam method
5.1.2.1 Principle
Dissolve the sample in sulfuric acid and ammonium sulfate, then add to dilute it, move the solution into the zinc amalgam reduction device, add zinc For amalgam reduction, use ammonium thiocyanate solution as indicator and titrate with ferric ammonium sulfate standard titration solution. 5.1.2.2 Reagent
5.1.2.2.1 Sulfuric acid (GB625); p1.84g/mL. 5.1.2.2.2 Sulfuric acid (GB625) solution: dilute 1+18. 5.1.2.2.3 Sulfuric acid (GB625) solution: dilute 1+45. 5.1.2.2.4 Sulfuric acid (GB625) solution: dilute 1+90. 5.1. 2.2.5 Ammonium thiocyanate indicator (GB660): 100g/L solution. 5.1.2.2.6 Ammonium sulfate (GB1396).
5.1.2.2.7 Carbon dioxide or nitrogen: in steel bottles. 5.1.2.2.8 Ferric ammonium sulfate standard titration solution: c[NH,Fe(SO,)]=0.06mol/L. Prepare according to 5.1.1.2.4, and calibrate according to 5.1.2.4.2 with 0.19~0.21g titanium dioxide standard reference material. 5.1.2.2.9 Zinc amalgam: 3% (m/m). Take 50mL of mercury, place it in small porcelain blood placed on the steam bath, cover the surface of the mercury with sulfuric acid solution (5.1.2.2.4), add 20~30g of small zinc particles, stir frequently, and add to dilute acid as needed Add water. When all the solid zinc has disappeared, allow the zinc amalgam to cool and sit for several hours. Finally, filter with Gustav without asbestos layer and store the zinc amalgam in a vial under the sulfuric acid solution (5.1.2.2.4). 50mL of this solution can be used for multiple reduction tests. When it fails, zinc can be added to activate it in the same way. 5.1.2.3 Instruments
5.1.2.3.1 Oven: capable of maintaining a temperature of 105110°C. 5.1.2.3.2 Balance: sensitivity 0.0001g. 5.1.2.3.3 Zinc amalgam reduction device: See Figure 2. 5.1.2.4 Operation steps
5.1.2.4.1 Sample
GB1706-93
Figure 2 Zinc amalgam Reduction device
a-ball tube, b, c, d-piston; e-funnel; f-hose g-flask Weigh the dried sample 0.19~0.21g, accurate to 0.0001g. 5.1.2.4.2 Determination
Place the sample in a 250mL beaker, add 20mL sulfuric acid (5.1.2.2.1) and 10g ammonium sulfate (5.1.2.2.6), mix carefully and cover with surface blood. Heat on an electric stove until thick smoke appears, and continue heating at low temperature until the sample is completely dissolved (usually boiling for a few minutes is completed), or until the remainder is completely composed of silica or silicon-containing substances. Cool the solution and dilute with 100 mL of water. If necessary, stir and filter, and wash the insoluble residue with cold sulfuric acid (5.1.2.2.2). Connect flask (g) to piston (d), with pistons (b) and (d) open, pour enough sulfuric acid solution (5.1.2.2.3) to fill flask (g) through funnel (e), And make sure there are no air bubbles left under the piston (d). Close the piston (d) and add 20mL of zinc amalgam (5.1.2.2.9) into the bulb (a) through the funnel (e) and piston (b). Heat the filtrate with a volume of no more than 300 mL to 50°C, pour it into funnel (e), connect piston (c) to the carbon dioxide source or nitrogen source, pass inert gas for 3 minutes, and close pistons (b) and (c). After removing the source of the erotic gas, remove the entire instrument fixed on the stand. With the pistons closed, hold the instrument and shake it vigorously for 5 minutes. After generating the characteristic purple color of trivalent titanium, hold the instrument vertically and open the piston (d ) and allow the zinc amalgam to flow into flask (g). Be careful when doing this! When the zinc amalgam passes, immediately close the piston (d), remove the flask (g) and the rubber tube (f) and save the zinc amalgam for next use. Then connect the gas supply pipeline to the inert gas, first open the piston (c), and then open the piston (b). Add 10 mL of ammonium thiocyanate (5.1.2.2.5) into the bulb (a), and titrate with ferric ammonium sulfate standard titration solution (5.1.2.2.8) until light orange appears, and keep it unchanged for 1 minute. To facilitate titration, a rubber tube can be used to connect a very narrow glass tube to the tip of the burette. This extension can pass through the piston (b) into the tube (a).
5.1.2.5 Expression of results
Titanium dioxide content, expressed as mass percentage, calculated according to formula (3): Tio.%=
0.0799Xc.V
m3
100
3
GB1706-93
Where: c—actual concentration of ferric ammonium sulfate standard titration solution, mol/L; V3—titration consumption of ferric sulfate Volume of ammonium standard titration solution, mL; mass of m3 sample, g;
0.0799—and 1.00mL ferric ammonium sulfate standard titration solution (c[NH,Fe(SO,),)=1.000mol/L ) is equivalent to the mass of titanium dioxide expressed in grams.
5.1.3 Allowable difference
The difference between two parallel measurements shall not be greater than 0.4%. 5.2: Comparison of colors
shall be carried out in accordance with the provisions of GB1864. The sample size is 2.00g, and the amount of refined linseed oil added is 0.8~1.1mL. 5.3 Comparison of achromatic power
shall be carried out in accordance with the provisions of GB5211.16.
5.4 Determination of volatile matter at 105℃
According to the regulations in GB5211.3.
5.5 After pretreatment for 24 hours at 23±2℃ and relative humidity (50±5)%, measurement of volatile matter at 105℃. Put about 30g of the sample into a loose mouth container, such as $70mm weighing Bottles or evaporating dishes (the thickness of the sample does not exceed 2cm) are placed in a constant temperature room at 23 ± 2°C and relative humidity (50 ± 5)%. After 24 hours, proceed according to the provisions of Article 5.4. If there is no constant temperature room, when the temperature is 23±2℃, the constant temperature and humidity conditions can be achieved according to the glycerin (glycerol) or chemical solution method in GB2424.2.
5.6 Determination of water-soluble substances
According to GB5211.The requirements in 2 are carried out, and the sample size is 10g. Note: If the pigment is highly dispersed, it can be measured as follows: weigh 5g of the sample, place it in a beaker, add 100mL of water, heat and boil for 5 minutes, cool, then add 25mL of 40g/L ammonium carbonate solution while stirring, and leave it for a while. , transfer the solution to a 250mL volumetric flask, dilute to the mark with water, and shake well. Filter through two layers of slow filter paper until a clear filtrate is obtained. Pipette 100 mL of filtrate into a weighing bottle and evaporate to dryness on a water bath. The following operations are still carried out in accordance with GB5211.2. A blank test was performed at the same time. The relative error of two parallel measurements shall not be greater than 8%. 5.7 Determination of pH value of water suspension
shall be carried out in accordance with the provisions of GB1717.
5.8 Determination of oil absorption
shall be carried out in accordance with the provisions of GB5211.15. The sample size is 5g. 5.9 Determination of sieve residue
shall be carried out in accordance with the provisions of GB5211.14. The sample amount is 20g, the dispersant is sodium hexametaphosphate, the concentration is 100g/L, and the adding amount is 3~5mL. 5.10 The measurement of resistivity of water extract
shall be carried out in accordance with the provisions of GB5211.12.
6 Inspection Rules
6.1 Before leaving the factory, titanium dioxide pigments should be inspected by the inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer should ensure that all manufactured products comply with the technical requirements of this standard. Each batch of products leaving the factory should be accompanied by a product grade certificate. 6.2 All technical requirements items listed in this standard are type inspection items, among which TiO2 content, color, achromatic power, 105°C volatile matter, water-soluble matter, water suspension pH value, oil absorption and sieve residue are factory inspection items . Under normal production conditions, the resistivity of the water extract solution should be tested at least once a month; the 105°C volatiles should be tested at least once a quarter after pretreatment for 24 hours. 6.3 Sampling method: According to the relevant regulations in GB9285. 6.4 The receiving department has the right to inspect the product in accordance with the provisions of this standard. If the quality is found not to meet the provisions of this standard, both the supply and demand parties shall jointly take double samples for re-inspection in accordance with the provisions of Article 6.3. If the quality still does not meet the provisions of this standard, According to regulations, the product is deemed to be defective. GB1706--93
6.5 When a dispute arises between the supply and demand parties on product quality, the product quality supervision and inspection agency shall conduct arbitration. 6.6 The determination of the inspection results in this standard shall be based on the rounded value comparison method in GB1250. 7 Logo, packaging, transportation, storage
7.1 Logo
The product packaging bag should be printed with a firm and clear mark, including the name of the manufacturer, product name, registered trademark, standard code, model, quality Grade, production batch number, net weight, production date and the specified "wet-afraid" mark 7.2 Packaging
The product should be packed in a plastic woven bag lined with plastic film bag, with a net weight of 25kg per bag. 7.3 Transportation
When transporting, loading and unloading, pack and unload lightly to prevent packaging contamination and damage. Products should be protected from rain and sunlight during transportation. 7.4 Storage
Products should be stored in ventilated and dry places according to grade, classification, and batches. Contact with items that may react with the product is strictly prohibited, and attention should be paid to moisture prevention. Additional instructions:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the National Coatings and Pigments Standardization Technical Committee. This standard is drafted by the Coatings Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Pei Lian'e, Zheng Wenjuan, Jin Liandi and Zhao Ling.
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