HG/T 2772-1996 Industrial zirconium oxychloride octahydrate (zirconium oxychloride)
Some standard content:
HG/T2772—1996
This standard is formulated based on the domestic main enterprise standards and has three levels. The difference from the enterprise standard is: referring to the Japanese standard JISK8210:1986 octahydrate zirconium oxychloride (reagent), three indicators of potassium oxide, calcium oxide and sulfate are added compared with the enterprise standard; the water-insoluble index is omitted, because this item is indirectly controlled in the main content determination, so it is no longer required in this standard.
This standard refers to the Japanese standard and adopts two measurement methods for the main content. 2
3The index parameters of the superior products of this standard are formulated with reference to the Japanese standard JISK8210:1986. The test methods of potassium oxide, calcium oxide and sulfate refer to the test methods of the Japanese standard; the test method of titanium dioxide adopts the method of GB/T2590.61981 national standard.
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Jiaozuo Chemical General Plant of Henan Province, and Yixing Chemical Plant of Jiangsu Xinxing Chemical Group Corporation.
The main drafters of this standard are: Liu Youruo, Zang Jincheng, Sun Yaguang, Yang Xinmin, Yang Fupei, and Yao Jinjuan. 247
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1 Scope
Chemical Industry Standard of the People's Republic of China
Industrial Zirconium Dichloride Octahydrate (Zirconium Oxychloride) HG/T 2772-—1996
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation, and storage of industrial zirconium dichloride octahydrate (zirconium oxychloride).
This standard applies to industrial zirconium dichloride octahydrate (zirconium oxychloride). This product is mainly used as a raw material for the manufacture of zirconium dioxide, an additive for the rubber and papermaking industries, a coating desiccant, and a treatment agent for refractory materials, ceramic glazes, and textile industries. Molecular formula: ZrOC12·8H20
Relative molecular mass: 322.25 (according to the 1991 international relative atomic mass) 2 Reference standards
The provisions 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 valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB 191 --.1990
Packaging, storage and transportation pictorial marking
Preparation of standard solutions for titration analysis (volume analysis) GB/T601-1988 Chemical reagents
GB/T 602--1988
GB/T 603—1988
GB,T 1250-
--1989
Chemical reagents
Preparation of standard solutions for determination of impurities (neqISO6353-1:1982) Preparation of preparations and products used in test methods (neqISO6353-1:1982) Chemical reagents
Methods for expressing and determining limit values GB/T 2590.1—1981
GB/T 2590.2—1981
GB/T 2590. 3—1981
GB/T 2590. 6—1981
GB/T 6678—1986
GB/T 6682—1992
GB/T 8946.-- 1988
3 Requirements
Determination of the total amount of zirconium oxide and hafnium oxide in zirconium oxide and hafnium oxide (mandelic acid weight method) Determination of the amount of iron in zirconium oxide and hafnium oxide (sulfosalicylic acid absorptiometry) Determination of the amount of silicon in zirconium oxide and hafnium oxide (silicon molybdenum blue absorptiometry) Determination of the amount of titanium in zirconium oxide and hafnium oxide (diantipyrine methane absorptiometry) General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (eqvISO) 3696: 1987) Plastic woven bags
Appearance: white or slightly yellow needle-shaped crystals. 3.12
3.2 Industrial octahydrate dichlorozirconium oxide shall meet the requirements of Table 1: Table 1 Requirements
Accounted in ZrOz
Main content
Accounted in Zr0Cl, · 8H20 Calculation
Iron oxide (Fe20) content
Approved by the Ministry of Chemical Industry of the People's Republic of China on January 24, 1996 248
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Superior product
Qualified product
Implemented on January 1, 1997
Silicon dioxide (SiO2) content
Sodium oxide (Naz2O3) content
Potassium oxide (KO2) content
Titanium dioxide (TiO2) content
Calcium oxide (CaO) content
Sulfate (measured in SO2) content
4 Sampling
4.1 Each batch of products shall not exceed 10t.
HG/T 2772--1996
Table 1 (end)
Superior products
First-class products
Qualified products
4.2 Determine the number of sampling units according to the provisions of GB/T66786.6. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the depth of the material layer to take samples. After mixing the collected samples, reduce them to no less than 500g according to the quartering method, and pack them into two clean and dry wide-mouth bottles with stoppers and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other bottle is kept for three months for reference. 4.3 If one of the test results does not meet the requirements of this standard, re-sample from twice the amount of packaging for verification. If even one of the verification results does not meet the requirements of this standard, the entire batch of products will be unqualified. 5 Test methods
5.1 All eight index items specified in this standard are type test items, among which the main content, iron oxide content, silicon dioxide content, sodium oxide content, and sulfate content are routine test items and should be tested batch by batch. Under normal production conditions, type tests are carried out every two months.
5.2 Use the rounding value specified in GB/T12505.2 to compare and determine whether the test results meet the standard. 5.3 The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and product used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602, and GB/T603. 5.4 Determination of main content
5.4.1 Method summary
Same as Chapter 1 of GB/T2590.1.
5.4.2 Reagents and materials
5.4.2.1 Hydrochloric acid solution: 1+1;
5.4.2.2 Silver nitrate solution: 10g/L;
Other reagents and materials are the same as those in Chapter 2 of GB/T2590.1. 5.4.3 Analysis steps
Weigh about 5g of sample (accurate to 0.0002g), place it in a 250ml beaker, add 50ml of water, and heat to dissolve. After cooling, transfer all to a 250mL volumetric flask, dilute to the mark with water, and shake well. Dry filter with qualitative analysis filter paper into a clean and dry 250mL beaker, and discard 20ml of the front filtrate.
Use a pipette to transfer 25.0ml of the above filtrate, place it in another clean 250mL beaker, add 30mL of water and 50mL of hydrochloric acid solution, heat to boiling, and remove. The following operations are carried out according to Chapter 3 of GB/T 2590.1, starting from “adding 50 ml of 16% bitter bean acid solution” to “burning in a high-temperature furnace at 900°C until constant weight”. 249
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5.4.4 Expression of analysis results
HG/T 2772—1996
The main content expressed in mass percentage (calculated as ZrO2) X1 is calculated according to formula (1): Xi = mi
m2×100
m×250
(ml-mz)×1 000
The main content expressed in mass percentage (calculated as ZrOCl2·8H2O) X is calculated according to formula (2): X2 = 2.615 2 XX
In the formula: mi--
The mass of the precipitate and the crucible, g;
The mass of the empty crucible, g;
The mass of the sample, g;
The coefficient for converting zirconium oxide into zirconium dichloride octahydrate. 2.615 2—
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.5% in terms of ZrOCl2·8H2O and 0.2%.
5.5 Determination of iron oxide content
5.5.1 Method summary
Same as Chapter 1 of GB/T2590.2.
5.5.2 Reagents and materials
Same as Chapter 2 of GB/T2590.2.
5.5.3 Analysis steps
5.5.3.1 Drawing of working curve
Draw according to Chapter 3 of GB/T2590.2.
5.5.3.2 Determination of sample
Weigh about 2g of sample (accurate to 0.01g), put it in a 100mL beaker, and add 20mL of water to dissolve. Heat slightly, and then follow Chapter 3 of GB/T2590.2 from "add 10mL25% sulfosalicylic acid solution..." to "find the corresponding iron content from the working curve". Perform a blank test at the same time. 5.5.4 Expression of analysis results
The iron oxide (Fe2O) content X expressed as mass percentage is calculated according to formula (3): (ml-mo) × 10- × 1. 430 × 100Xa
_ (ml-mo) X 10-^ × 1. 430
Wherein: mo-
the amount of iron in the blank test obtained from the working curve, μg; the amount of iron in the sample obtained from the working curve, ug; 1.430-——the coefficient for converting iron into ferric oxide; m--
the mass of the sample, g.
5.5.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0005%. 5.6 Determination of silicon dioxide content
5.6.1 Summary of the method
Same as Chapter 1 of GB/T2590.3.
5.6.2 Reagents and materials
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·(3)
Same as Chapter 2 of GB/T2590.3.
5.6.3 Analysis steps
5.6.3.1 Drawing of working curve
HG/T 2772—1996
Weigh 4.00g of sample (accurate to 0.01g), place it in a 200ml beaker, add water to dissolve. Transfer all to a 100ml volumetric flask, dilute to the mark with water, and shake to hook. Take 10ml of each sample and place them in 6 polyethylene beakers. Add 20 drops of hydrofluoric acid, heat in a boiling water bath for 5 minutes, and cool. The following operations are carried out according to the "dilute with water to 60ml" in the working curve drawing of Chapter 3 of GB/T2590.3, and end with the drawing of the working curve.
5.6.3.2 Determination of the sample
Weigh about 0.5g of the sample (accurate to 0.01g), place it in a 150mL plastic beaker, moisten it with water, add 20 drops of hydrofluoric acid, heat in a boiling water bath for 5 minutes, and add water to 60mL. The following determination is carried out according to Chapter 3 (1) of GB/T2590.3 starting from "add 2.5g of boric acid...". Perform a blank test at the same time.
5.6.4 Expression of analytical results
Silicon dioxide (SiO2) content X expressed as mass percentage. Calculate according to formula (4): Xx (m=mo)×10×2.139×100
_ (ml=mo)×10-1×2.139
wherein m-the amount of silicon in the blank test obtained from the working curve, ug; m-the amount of silicon in the sample obtained from the working curve, ug; 2.139-…--the coefficient for converting silicon into silicon dioxide; m---the mass of the sample, g.
5.6.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.005%. 5.7 Determination of sodium oxide and potassium oxide content
5.7.1 Summary of method
Dissolve the sample in water, and use the standard addition method on a flame photometer or an atomic absorption spectrophotometer with flame emission to measure the spectral intensity of sodium and potassium excited by flame combustion at wavelengths of 589.0nm and 766.5nm, respectively, and calculate the content of sodium oxide and potassium oxide.
5.7.2 Reagents and materials
Sodium and potassium standard solution: 1ml. The solution contains 10ug sodium and 10μg potassium. Take 10.0mL of sodium standard solution and potassium standard solution prepared according to GB/T602, respectively, place them in a 100mL volumetric flask, dilute to the scale with water, and shake well. The solution is prepared before use. 5.7.3 Instruments and equipment
Flame photometer or atomic absorption spectrophotometer with flame emission. 5.7.4 Analysis steps
Weigh 0.5g~2.0g of sample (accurate to 0.001g) and place it in a 100mL beaker. Add 30mL of water, transfer to a 100mL volumetric flask, add water to the mark, and shake well.
Pipette 10.0ml of the above solution respectively, place it in 4 clean volumetric flasks, add 0.00, 1.00, 2.00, 3.00ml of sodium and potassium standard solutions respectively, add water to the mark, and shake well. On a flame photometer or an atomic absorption spectrophotometer with flame emission, measure the radiation intensity at a wavelength of 589.0nm for sodium and 766.5nm for potassium. Draw a curve with the sodium and potassium content of the added standard solution as the horizontal axis and the corresponding absorbance as the vertical axis. Extend the curve in the opposite direction to intersect with the horizontal axis. The intersection point is the content of the test solution to be determined. 5.7.5 Expression of analysis results
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HG/T 2772—1996
Sodium oxide (Na2O) content X expressed in mass percentage: calculated according to formula (5): Xs
m X 1. 348
m×100
m×1. 348
Potassium oxide (KzO) content X expressed in mass percentage. Calculate according to formula (6): m2×1. 205
m2×1.205
Wherein: m-
1. 205 ---
The amount of sodium obtained by the curve extension, ug;
The amount of potassium obtained by the curve extension, ug;
The coefficient of sodium converted to sodium oxide;
The coefficient of potassium converted to potassium oxide;
The mass of the sample, g.
5.7.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.002%. 5.8 Determination of titanium dioxide content
5.8.1 Summary of method
Same as Chapter 1 of GB/T2590.6.
5.8.2 Reagents and materials
Same as GB/T2590.6 Chapter 2.
5.8.3 Analysis steps
5.8.3.1 Drawing of working curve
Perform according to G1B/T2590.6 Chapter 3 “Drawing of working curve”. (5)
·（6)
5.8.3.2 Determination of sample
Weigh about 3g of sample (accurate to 0.01g) and place it in a 100mL beaker. The following is in accordance with GB/T2590.6 Chapter 3 starting from “add 7mL10% oxalic acid solution·” to “find the corresponding titanium content from the working curve”. 5.8.4 Expression of analysis results
The titanium dioxide (TiO2) content X expressed as a mass percentage is calculated according to formula (7): X, = mi × 10-° × 1. 668
_m × 10- × 1. 668
Wu Zhong: m
—…the amount of titanium found from the working curve, ug; 1.668--the coefficient for converting titanium into titanium dioxide; m-the mass of the sample, g.
5.8.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0001%. 5.9 Determination of calcium oxide content
5.9.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer using a wavelength of 422.7nm and an air-acetylene flame. 5.9.2 Reagents and materials
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HG/T 2772—1996
Calcium standard solution: 1mL solution contains 0.1mgCa. 5.9.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a calcium hollow cathode lamp. 5.9.4 Analysis steps
Weigh 1.00g sample (accurate to 0.01g) and place it in a 100mL beaker. .After dissolving in water, transfer to a 100mL volumetric flask, add water to the mark, and shake well. As solution X. Weigh another 1.00g sample (accurate to 0.01g) and place it in a 100ml.beaker. After adding a small amount of water to dissolve, use a pipette to add calcium standard solution as follows, transfer to a 100ml volumetric flask, add water to the scale, and shake it. As solution Y. On an atomic absorption spectrophotometer, use a wavelength of 422.7nm line and an air-acetylene flame to measure the absorbance of solution X (A,) and solution Y (A,) respectively.
Where A is not greater than (A2A), it is qualified. Calcium standard solution should be added according to the following regulations: superior product: 1.00mL,
---quality product: 2.00 mL;
Qualified product: 3.00mL.
5.10 Determination of sulfate content
5.10.1 Summary of method
Dissolve the sample in water, add barium chloride solution in an acidic medium, produce a white precipitate of barium sulfate, and compare it with the standard turbidimetric solution treated at the same time by visual turbidimetry. bzxz.net
5.10.2 Reagents and materials
5.10.2, 195% ethanol;
5.10.2.2 Hydrochloric acid solution: 1+1;
5.10.2.3 Barium chloride solution: 100g/1; 5.10.2.4 Sulfate standard solution: 1mL solution contains 0.1mgSO4. 5.10.3 Analysis steps
Weigh 2.00g of sample (accurate to 0.01g), place in a 50mL colorimetric tube, add 0.4mL hydrochloric acid solution and 25mL water to dissolve, add 3mL. 95% ethanol, 2ml. Barium chloride solution, let stand for 30min, the white turbidity produced shall not be darker than the standard turbidity solution. The standard turbidity solution is to transfer the sulfate standard solution according to the following regulations, and treat it in the same way as the sample. Superior product: 1.0ml;
First-class product: 1.6 mL;
Qualified product: 2.0ml.
6 Marking, packaging, transportation, storage
6.1 Industrial zirconium oxychloride octahydrate should have firm and clear markings on the packaging, including: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "heat-afraid" and "humidity-afraid" marks specified in GB191. 6.2 Each batch of industrial zirconium oxychloride octahydrate shipped from the factory should be accompanied by a quality certificate. The contents include: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and this standard number. 6.3 Industrial zirconium oxychloride octahydrate is packaged in three layers. The inner packaging adopts two layers of polyethylene plastic film bags, the thickness of which shall not be less than 0.05mm; the outer packaging adopts plastic woven bags, the performance and inspection methods of which shall comply with the provisions of Type B of GB/T8946. The net weight of each bag is 50kg. 6.4 For the packaging of industrial zirconium oxychloride octahydrate, the inner bag is tied tightly with two layers of vinyl rope or other ropes of equivalent quality, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the edge of the bag, and the opening is sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the edge of the bag. The stitch length is 7mm~12mm, the stitches are neat and uniform, and there is no leakage or skipping. 6.5 Industrial zirconium oxychloride octahydrate should be covered during transportation to prevent rain and moisture. 6.6 Industrial zirconium oxychloride octahydrate should be stored in a cool and dry place to prevent rain and moisture. 253
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