Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2308-92
Published on May 17, 1992
Floatation Agent
Implemented on January 1, 1993
Ministry of Chemical Industry of the People's Republic of China
W Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG/T2308-92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of GF flotation agent. This standard applies to the flotation agent obtained by saponification and precipitation separation of the residual liquid in the production process of butyl octanol. The main components are CC: higher alcohols, esters, hydrocarbons and a small amount of aldehydes, acids and other organic compounds that are effective flotation ingredients. 2
Cited standards
GB1250bZxz.net
GB4472
GB4757
GB6678
GB8170
3 Technical requirements
3.1 Appearance
Packaging Storage and transportation Pictorial signs
Preparation of standard solutions for chemical reagent titration analysis (volume analysis) Preparation of preparations and products used in chemical reagent test methods Methods for expressing and determining limit values General rules for determination of density and relative density of chemical products Unit flotation test method for coal preparation laboratories
General rules for sampling of chemical products
Rules for rounding off values
Orange-yellow to dark brown oily liquid.
3.2GF flotation agent shall meet the requirements in the following table.
Density p20g/cm3
Hydroxyl value, mgKOH/g
Saponification value, mgKOH/g
Residual liquid, %(V/V）
4Test method
First-class product
0.870~0.900
Qualified product
Unless otherwise specified, the reagents and water used in this test method are analytical reagents and distilled water or water of equivalent purity. Unless otherwise specified, the standard solution preparations and products used in this standard are prepared in accordance with GB601 and GB603. Approved by the Ministry of Chemical Industry of the People's Republic of China on May 17, 1992 and implemented on January 1, 1993
W.4.1 Determination of density
4.1.1 Analysis steps
HG/T2308-92
Determination temperature: 20℃. Use a density meter marked with a scale for reading the upper edge of the meniscus. Determine according to the density meter method in Article 2.3.3 of GB4472.
Take the arithmetic mean as the determination result.
4.1.2 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.001g/cm. 4.2 Determination of hydroxyl value
4.2.1 Principle of the method
Alcohol reacts with excess acetylating agent. After the reaction is completed, water is added to hydrolyze the remaining acetic anhydride, and then the generated acetic acid is neutralized with alkali.
4.2.2 Reagents and solutions
4.2.2.1 n-Butanol;
4.2.2.2 Acetylation agent: Measure 45mL of pyridine and place it in a 100mL dry conical flask with a glass stopper, add 0.5mL of 70%72% perchloric acid, add 10mL of acetic anhydride and mix well, prepare temporarily when using; 4.2.2.3 Sodium hydroxide ethanol standard titration solution: c(NaOH)-0.5mol/L, weigh 20.0g of sodium hydroxide, dissolve it in 30mL of water, dilute it to 1000mL with anhydrous ethanol, let it stand for 24h, take the clear solution and calibrate it according to GB601; 4.2.2.4 Cresol red-bromothymol blue mixed indicator: Cresol red ethanol solution (1g/L) and bromothymol blue ethanol solution (10g/L) are mixed in a ratio of 1+3.
4.2.3 Analysis steps
Weigh 0.5g of the sample, accurate to 0.0001g, put it into a 100mL iodine volumetric flask, add 5mL of acetylating agent, cover the bottle stopper tightly, and heat it in a boiling water bath for 30min. After cooling, add 10mL of water, then rinse the bottle stopper and bottle wall with 10mL of n-butanol, add 6 drops of mixed indicator, and titrate with sodium hydroxide ethanol standard titration solution until the color changes from yellow to blue as the end point. At the same time, perform a blank test. 4.2.4 Result calculation
The hydroxyl value X1 (mgKOH/g) is calculated according to formula (1): Xi=(.-V)) :ciX0. 056 1)
Where: V. Blank consumption of sodium hydroxide ethanol standard titration solution, mL; V1——Volume of sodium hydroxide ethanol standard titration solution consumed by the sample, mL; ci——Actual concentration of sodium hydroxide ethanol standard titration solution, mol/L; -Mass of the sample, g;
0.0561——Mass of potassium hydroxide expressed in grams equivalent to 1.00ml sodium hydroxide ethanol standard titration solution [c (NaOH) = 1.000mol/L].
Take the arithmetic mean of two parallel determinations as the determination result. 4.2.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 8mgKOH/g. 4.3 Determination of saponification value
4.3.1 Principle of the method
Excess alkali neutralizes the acid in the sample and reacts with the esters in the sample for saponification. After the reaction is completed, the remaining alkali is neutralized with acid. 4.3.2 Reagents and solutions
4.3.2.1 Anhydrous ethanol;
4.3.2.2 Potassium hydroxide ethanol solution: c(KOH)=0.5mol/L;2
HG/T2308—92
4.3.2.3 Standard hydrochloric acid titration solution: c(HCI)=0.5mol/L; 4.3.2.4 Bromothymol blue indicator solution: 1g/L. 4.3.3 Analysis steps
Weigh 0.5g of the sample, accurate to 0.0001g, and place it in a 250mL ground-mouth conical flask. Add 25.0mL of potassium hydroxide ethanol solution accurately, connect the condenser to a boiling water bath, heat and reflux for 1h, cool slightly, rinse the condenser with 5mL of anhydrous ethanol, remove the conical flask, add 8 drops of bromothymol blue indicator solution, and titrate with hydrochloric acid standard titration solution until the solution changes from blue to yellow, which is the end point. Perform a blank test at the same time.
4.3.4 Calculation of results
The saponification value X (mgKOH/g) is calculated according to formula (2): X: (V.V) #c×0. 056 1×1000
Where: V. ——Blank volume of hydrochloric acid standard titration solution consumed, mL; V2—volume of hydrochloric acid standard titration solution consumed by the sample, mL; C2
—actual concentration of hydrochloric acid standard titration solution, mol/L; m——mass of the sample, g;
0.0561——mass of potassium hydroxide expressed in grams equivalent to 1.00mL hydrochloric acid standard titration solution [c(HC1)=1.000mol/L).
Take the arithmetic mean of two parallel determinations as the determination result. 4.3.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 8mgKoH/g. 4.4 Determination of residual liquid
Take 100mL of the mixed sample and inject it into the Rissenk bottle. After it is placed at room temperature for 1h and naturally settled, visually observe the volume of the residual liquid. 4.4.1 Result calculation
Residual liquid volume percentage X: Calculate according to formula (3): Vs
Wherein: Vs—visual residual liquid volume, mL; 100—sample volume, mL.
5 Inspection rules
(3)
5.1GF flotation agent products should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that each batch of products shipped out of the factory meets the requirements of this standard.
5.2Each batch of GF flotation agent shipped out of the factory should be accompanied by a quality certificate in a certain format. The content includes: manufacturer name, product name, batch number, production date, product quality grade and standard number of this product. 5.3 For GF flotation agents loaded in tank trucks, each tank truck is considered as a batch, and the sampler is used to take average samples from the upper, middle and lower layers. For barreled GF flotation agents, each finished product purchased tank is considered as a batch. The sampling quantity shall be carried out in accordance with the requirements of Table 2 in GB6678, and the sampling method shall be carried out in accordance with Article 2.1.3 in GB6680.
5.4 The total amount of the sample shall not be less than 1L. After the sample is fully mixed, it shall be divided into two clean and dry glass bottles with ground stoppers. Labels shall be attached and the manufacturer's name, product name, batch number, sampling date and sampler shall be indicated. One bottle shall be used for inspection and analysis, and the other bottle shall be sealed and kept for one month for inspection.
5.5 The user has the right to re-inspect the quality of the GF flotation agent products received in accordance with the inspection rules and test methods specified in this standard to re-inspect whether its quality meets the requirements of this standard. HG/T2308—92
5.6 When the production and use units inspect the products, if one of the indicators does not meet the requirements of this standard, the tank truck products should be re-sampled from twice the number of packages, and the barreled products should be re-sampled from twice the number of packages for inspection. If one of the indicators obtained does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.7 When the supply and demand parties have disputes over product quality, they shall be resolved through negotiation, or arbitration shall be conducted in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
5.8 When determining whether the test data meets the technical indicators specified in the standard, the rounded value comparison method of GB1250 shall be used, and the rounding shall be carried out in accordance with GB8170.
5.9 If the user has requirements for the unit flotation test, it shall be measured according to the GB4757 method, and the indicators shall be determined by negotiation between the supply and demand parties. 6 Marking, packaging, transportation and storage
6.1 On the packaging container of GF flotation agent products, a firm mark should be painted, which includes the product name, this standard number, quality grade, trademark, manufacturer name, batch number, net weight and the "heat-afraid" and "wet-afraid" marks in Figure 4 and Figure 7 of GB191. 6.2 GF flotation agent should be packaged in clean tank trucks and firm iron barrels, with a net weight of 150kg per barrel. 6.3 Avoid violent impact during loading, unloading and transportation. 6.4 GF flotation agent products should be stored in a cool and dry warehouse, prevent exposure to sunlight and rain, and avoid contact with open flames. Additional remarks:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Beijing Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Changsong Chemical Plant of Jilin Chemical Industry Corporation. The main drafter of this standard is Zhang Min.
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