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GB 28655-2012: [GB/T 28655-2012] Ammonium bifluoride for industrial use
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[GB/T 28655-2012] Ammonium bifluoride for industrial use
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Basic data | Standard ID | GB 28655-2012 (GB28655-2012) | | Description (Translated English) | [GB/T 28655-2012] Ammonium bifluoride for industrial use | | Sector / Industry | National Standard | | Classification of Chinese Standard | G12 | | Classification of International Standard | 71.060.50 | | Word Count Estimation | 9,926 | | Quoted Standard | GB 190-2009; GB/T 191-2008; GB/T 6678; GB/T 6682-2008; GB/T 8170; HG/T 3696.1; HG/T 3696.2; HG/T 3696.3 | | Regulation (derived from) | National Standards Bulletin No. 24 of 2012 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the requirements of industrial ammonium bifluoride, test methods, inspection rules, marking, labeling, packaging, transportation, storage, and security. This standard applies to industrial hydrofluoric acid and ammonia in t | GB 28655-2012: [GB/T 28655-2012] Ammonium bifluoride for industrial use---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Ammonium bifluoride for industrial use
ICS 71.060.50
G12
National Standards of People's Republic of China
Industrial ammonium hydrogen fluoride
Published 2012-09-03
2013-06-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
8.1,8.3,8.4,8.5 this standard Chapter 7, Chapter 8, Chapter 9 is mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
The standard proposed by China Petroleum and Chemical Industry Federation.
This standard by the National Standardization Technical Committee chemical inorganic chemicals branch (SAC/TC63/SC1).
This standard was drafted. Fluoride Chemicals Co., Ltd., Fujian Shaowu Yong Fei Chemical Co., Ltd., Zhejiang Chemical Co., fluorescent
The company, Zhejiang three US Chemical Co., Ltd., Zhejiang Ying Peng Chemical Co., Ltd., CNOOC Tianjin Chemical Research & Design Institute.
The main drafters. Yang Huachun, Wan group level, Guo Liming, Xu Yihong, Xie Friends of flood, He Zhengping Liu Ruo, Guo Fengxin.
Industrial ammonium hydrogen fluoride
1 Scope
This standard specifies the requirements of industrial ammonium hydrogen fluoride, test methods, inspection rules, marking, labeling, packaging, transportation, storage, and security.
This standard applies to industrial hydrofluoric acid and ammonia in a liquid phase under the reaction conditions and obtained, primarily as oil extraction solution blocking agent, fine ceramic
Industrial ammonium bifluoride porcelain filling additives, surface treatment of metals, glass products like etchant.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
GB 190-2009 dangerous goods packaging logo
GB/T 191-2008 Packaging Pictorial signs
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6682-2008 specifications and test methods for water analysis laboratory
GB/T 8170 rounding off means about rules and determining limiting values
Preparation HG/T 3696.1 Inorganic chemicals for chemical analysis of standard titration solution
Preparation HG/T 3696.2 Inorganic chemicals solution used for chemical analysis of standard impurities
Preparations with HG/T 3696.3 Inorganic chemicals Chemical Analysis
Molecular formula and molecular weight 3
Molecular formula. NH4HF2
Molecular weight. 57.04 (according to 2007 international relative atomic mass)
4 Requirements
4.1 Appearance. white crystal.
4.2 ammonium hydrogen industry should meet the requirements of Table 1.
Table 1
project
index
Premium grade First grade Qualified
Ammonium bifluoride (of NH4HF2) (dry basis) w /% ≥ 98.0 97.0 96.0
Ammonium fluorosilicate [(NH4) 2SiF6] w /% ≤ 0.5 1.5 3.0
Loss on drying w /% ≤ 1.5 3.0 4.0
Residue on ignition w /% ≤ 0.1 0.2 -
Sulfate (in terms of SO4) w /% ≤ 0.1 0.1 -
5 Test methods
5.1 Safety Tips
Ammonium bifluoride in this test method the sample taken toxic, deliquescent in the air and the solution is strongly acidic, during operation
Try not to be in direct contact with the skin. Reagents used is corrosive, the operator should be careful to avoid contact with the skin, such as
Contact with the skin immediately wash with water, severe cases should seek medical care immediately.
5.2 General Provisions
This standard reagents and water, in the absence of other requirements specified, refer to three predetermined analytical reagents and GB/T 6682-2008 of
Water, used in the test standard titration solution, impurity standard solution, formulations and products, in the absence of other requirements specified, are by HG/T 3696.1,
HG/T 3696.2, preparing a predetermined HG/T 3696.3 is.
5.3 Visual inspection
Determined by visual appearance in natural light.
5.4 Determination of the content of ammonium bifluoride
5.4.1 Method summary
Under the temperature of 0 ℃, was added a saturated solution of potassium nitrate, in a sample to eliminate the interference of ammonium fluorosilicate, bromine thymol blue - neutral red is
Indicator, titrated titrated with standard sodium hydroxide solution.
5.4.2 Reagents and materials
5.4.2.1 saturated potassium nitrate solution.
5.4.2.2 sodium hydroxide standard titration solution. c (NaOH) ≈0.5mol/L.
5.4.2.3 Bromothymol Blue - neutral red mixed indicator solution.
Weigh 0.1g 0.1g of bromothymol blue and neutral red, was dissolved in ethanol 200mL95%.
5.4.2.4 ice. prepared with distilled or deionized water.
5.4.3 Analysis of step
Weigh about 0.8g sample by 5.6 after drying, the nearest 0.0002g, with a small amount of cold water to transfer the sample to a pre-filled with 20mL
Polyethylene beaker, 50g of potassium nitrate and a saturated solution of crushed ice, and stirred to dissolve the sample. Add 5 drops of bromothymol blue - mixing neutral red
Indicator solution, dark green end point titration with standard sodium hydroxide solution to titrate. After the titration solution is mixed with ice water to maintain a state immediately used
Determination of the content of ammonium fluoride.
5.4.4 calculation results
Ammonium fluoride ammonium hydrogen fluoride content (of NH4HF2) w1 mass fraction basis, calculated according to formula (1).
w1 =
(V/1000) cM
m × 100%
(1)
Where.
Sodium hydroxide standard titration solution volume V --- titration test solution consumed value in milliliters (mL);
Accurate value of the concentration of the solution of sodium hydroxide standard titration --- C, in units of moles per liter (mol/L);
Value m --- mass of the sample in grams (G);
--- numerical molar mass M ammonium bifluoride (NH4HF2), in units of grams per mole (g/mol) (M = 57.04).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to not more than 0.3%.
5.5 Determination of the content of ammonium fluorosilicate
5.5.1 Method summary
After determination of the content of ammonium fluoride was subjected to suction filtration in the cold state. At 80 ℃, fluorine potassium silicate precipitate was dissolved, to
Phenolphthalein as an indicator, titration is titrated with standard sodium hydroxide solution.
5.5.2 Reagents
5.5.2.1 chloride ethanol solution.
Weigh about 2g of potassium chloride dissolved 100mL50% ethanol.
5.5.2.2 sodium hydroxide standard titration solution. c (NaOH) ≈0.1mol/L.
5.5.2.3 phenolphthalein indicator solution. 10g/L.
5.5.3 instruments and equipment
5.5.3.1 polyethylene funnel.
5.5.3.2 polyethylene beaker.
5.5.3.3 constant temperature water bath. capable of controlling a temperature of 80 ℃ ~ 85 ℃.
5.5.4 Analysis of step
5.4.3 Determination solution was filtered through a polyethylene funnel and slow quantitative filter paper, held by suction filtration at 0 ℃ close state. With pre
KCl was washed thoroughly with ethanol cooled to precipitate, the precipitate together with the original filter into a beaker together. Adding about 100mL temperature
Of water, heated on a water bath to 80 ℃, add 5 drops of phenolphthalein indicator solution, titrated with standard sodium hydroxide solution was titrated to light red solution.
5.5.5 calculation results
Content fluorosilicate, ammonium fluorosilicate, ammonium [(NH4) 2SiF6] w2 mass fraction basis, according to equation (2).
w2 =
(V/1000) cM
m × 100%
(2)
Where.
Sodium hydroxide standard titration solution volume V --- titration test solution consumed value in milliliters (mL);
Accurate value of the concentration of the solution of sodium hydroxide standard titration --- C, in units of moles per liter (mol/L);
Value m --- mass of the sample in grams (G);
--- M ammonium fluorosilicate [14
Numerical 2SiF6] molar mass (NH4), in units of grams per mole (g/mol) (M = 44.54).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to no greater than 0.1%.
5.6 Determination of loss on drying
5.6.1 Method summary
The sample was dried in a silica gel desiccator, loss on drying is determined according to the reduction of the sample before and after drying.
5.6.2 instruments and equipment
5.6.2.1 platinum (or polytetrafluoroethylene) crucible.
5.6.2.2 Silicone dryer. indicator using silica gel desiccant.
5.6.3 Analysis of step
Weigh about 1g sample, accurate to 0.0002g, was placed on a silica gel dryer to a constant mass in a covered platinum (or PTFE
Ethylene) crucible, placed in a silica gel desiccator, and dried to open the lid of the crucible, placed immediately weighed 8h, fluorinated sample after drying
Determination of ammonium hydrogen content.
5.6.4 calculation results
Loss on drying w3 mass fraction basis, calculated according to formula (3).
w3 = m1-m2m × 100%
(3)
Where.
Numerical sample before drying and M1 --- crucible crucible mass in grams (G);
--- M2 dried sample values and quality of the crucible crucible in grams (G);
Value m --- mass of the sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to not more than 0.2%.
Determination of ignition residue content of 5.7
5.7.1 Method summary
The sample was fired in a high temperature furnace to constant mass, determined according to the ignition residue content reduction before and after burning.
5.7.2 instruments and equipment
5.7.2.1 platinum dish.
5.7.2.2 temperature furnace. temperature control can 700 ℃ ± 25 ℃.
5.7.3 Analysis of step
Weigh about 5g sample, accurate to 0.0002g, was placed at 700 ℃ ± 25 ℃ to constant mass burning platinum dish in ventilated
Good ventilation hood, slowly heated to complete the volatiles were evaporated. The platinum dish was placed 700 ℃ ± 25 ℃ high temperature burning furnace to constant mass.
5.7.4 calculation results
Residue on ignition w4 mass fraction basis, calculated according to formula (4).
w4 = m1-m2m × 100%
(4)
Where.
The residue on ignition values after M1 --- quality and platinum dish in grams (G);
Numerical empty platinum dish mass m2 ---, in grams (G);
Value m --- mass of the sample in grams (g).
Parallel to the arithmetic average of the measurement results of the measurement result, the absolute difference determination results parallel to 0.02%.
5.8 Determination of the sulfate content
5.8.1 Method summary
Hydrochloric acid and sodium carbonate solution was added a small amount in a sample, again evaporated to dryness on a water bath. After the residue was dissolved barium chloride solution of sulfuric acid
Salt precipitation as barium sulfate, turbidity standard for comparison.
5.8.2 Reagents
5.8.2.1 95% ethanol.
5.8.2.2 hydrochloric acid solution. 21.
5.8.2.3 sodium carbonate solution. 100g/L.
5.8.2.4 barium chloride solution. 100g/L.
5.8.2.5 sulfate standard solution. 1mL solution containing sulfate (SO4) 0.1mg.
Pipette with a pipette 10mL sulfate standard solution according to GB/T 3696.2 formulated, a 100mL volumetric flask, dilute with water
To the mark.
5.8.3 Analysis of step
0.50g ± 0.01g sample is weighed, placed in a platinum dish, the following operations carried out in a well ventilated hood was added 0.5mL carbonate
Sodium, 10 mL hydrochloric acid solution, evaporated to dryness on a water bath. After the operation was repeated three more times, with about 1mL 20mL aqueous hydrochloric acid solution
The residue was dissolved, the solution was transferred to a 100mL volumetric flask, diluted with water to the mark.
Pipette with a pipette 20mL of the solution (filtered if necessary), a 50mL colorimetric tube, add water to 25mL, was added 3mL
95% ethanol and 2mL barium chloride solution, allowed to stand 1h turbidimetry, turbidity should not be deeper than the standard turbidimetric solution.
Turbidity standard solution was prepared ratio. 0.3mL was added a sodium carbonate solution, 6 mL solution of hydrochloric acid in a porcelain evaporating dish, evaporated on a water bath to
dry. The residue was dissolved with a small amount of water and 0.2mL of hydrochloric acid solution, and the solution was transferred to a 50mL colorimetric tube, labeled sulfate was added 1.00mL
Standard solution, from the "25 mL water was added to the" start, and treated in the same sample simultaneously.
6 Inspection Rules
All items specified in 6.1 standard factory inspection items should be tested batches.
6.2 the same material, substantially same production conditions, the same team or continuous production of ammonium bifluoride industrial production batch. Each batch of products
Not more than 30t.
Unit 6.3 determines the number of samples required to GB/T 6678. Sampling the hard plastic tube sampler from above obliquely inserted into the packaging bag layers
3/4 sampling depth. The sample was placed in a sealed collection container, mixing, reduced to less than 500g, dispensed into a clean, dry two
Plastic bottle, sealed. Attach a label on the bottle, indicating manufacturer name, product name, grade, batch number, date of sampling and sample's name. For a bottle
Laboratory samples, another bottle stored for future reference, save time determined by the manufacturer according to the actual situation.
6.4 If the test results do not meet the requirements of this standard indicators, should be re-double the amount of self-packaging sampling retest, retest results even
Only when an indicator does not meet the requirements of this standard, the entire batch of product is substandard.
6.5 according to GB/T 8170 rounding predetermined value comparison determination whether or not the test results standard.
7 signs, labels
7.1 Industrial hydrogen fluoride should be a clear sign of the strong ammonium package, including. manufacturer's name and address, product name, grade, net weight, batch
Number (or date of manufacture), "toxic substances", and the predetermined standard number GB 190-2009 label, GB/T 191-2008 predetermined "fear
Sun "," afraid of the rain "logo.
7.2 Each batch of ammonium hydrogen fluoride industrial factory should be accompanied by a certificate of quality. They include. manufacturer's name and address, product name, grade, containing a net
Quantity, batch number (or date of manufacture) and the standard number.
8 packaging, transport and storage
8.1 packaging industry uses a two ammonium bifluoride. Polyethylene plastic film packaging bags; outer plastic bags.
8.2 net weight 25kg, or according to user requirements negotiated net content.
8.3 Industrial ammonium hydrogen fluoride package, the inner four artificial Zhakou with Vinyl rope or other comparable quality rope, or its equivalent with other parties
Sealing; packaging sewn securely, and not leaky jumper phenomenon.
8.4 during the transportation industry ammonium bifluoride should be covered, the temperature should not exceed 50 ℃, to prevent the sun, rain, moisture; not with acid, alkali
Mixed transportation.
8.5 Industrial ammonium bifluoride should be stored in a cool warehouse dedicated hazardous chemicals, the temperature should not exceed 50 ℃, to prevent the sun, rain and damp;
Not with acid, alkali mixed storage.
9 Security
9.1 ammonium bifluoride in the air easily deliquescence, easily soluble in water, acidic aqueous solution. Thermal decomposition of the toxic ammonia and hydrogen fluoride gas.
Production process should be closed operation, enhance ventilation. Workplace should be equipped with safety shower and eyewash equipment.
9.2 ammonium hydrogen fluoride to the skin, mucous membrane irritation. Contact with the skin can cause serious burns, inhalation irritation to the respiratory tract. Operator
Members should wear safety glasses, wear protective overalls and protective gloves. Emergency rescue or evacuation, should wear protective masks filter type
Or self-contained breathing apparatus.
9.3 ammonium bifluoride should be loaded and unloaded lightly handling, packaging and to prevent breakage of the container. To avoid dust, should not be in contact with an acid, a base.
9.4 ammonium bifluoride should be in direct contact with the skin. If you come into contact with skin, wash immediately with plenty of water, severe cases should seek medical care immediately.
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