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Chemical Industry Standard of the People's Republic of China
HG/T 2424 --93
Calcium stearate (light)
Published on March 10, 1993
Ministry of Chemical Industry of the People's Republic of China
Implementation on January 1, 1994
Chemical Industry Standard of the People's Republic of China
Calcium stearate (light)
1 Subject content and scope of application
HG/T 2424 — 93
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of calcium stearate products. This standard applies to calcium stearate obtained by double decomposition reaction of industrial stearic acid with calcium salt after saponification. This product is mainly used as a stabilizer and lubricant for polyoxyethylene.
Structural formula: RCOOC&OOCR (R is the mixed alkyl group in industrial stearin)2 Reference standard
GB 601
GB 603
GE 617
Chemical reagents
Preparation of standard solvents for titration analysis (volume analysis) Chemical reagents
Preparation of preparations and products used in test methods Melting point range of chemical reagents General test methods GB/T6678 General rules for sampling of chemical products
GB6682 Specifications and test methods for water used in analytical laboratories 3 Technical requirements
Appearance: white powder, without obvious mechanical impurities 3.1
Technical indicators
Calcium stearate should meet the requirements of the following table
Calcium content, %
Free acid (calculated as stearic acid), %
Heating loss, %
Melting point,
Fineness (passing 0.075 mm sieve), %
Bulk density, g/cm*
Test method
Superior product
6. 5±0. 5
149~155
First-class product
6. 5± 0. 6
Qualified product
6. 5± 0. 7
The standards, preparations and products used in this standard shall be prepared in accordance with the provisions of GB601 and GB603 unless otherwise specified.
Approved by the Ministry of Chemical Industry of the People's Republic of China on March 10, 1993, and implemented on January 1, 1994
HG/T 2424 —93
The water used in this standard shall comply with the specifications of Grade 3 water in GB6682 unless otherwise specified. 4.1 Determination of appearance
4. 2 Determination of calcium content
4.2.1 Experimental principle
The sample is decomposed into stearic acid and the corresponding calcium salt in a strong acid, and the calcium content is determined by complexation with disodium ethylenediaminetetraacetic acid standard titration solution 4.2.2 Reagents and solutions
Nitric acid (GB626) solution: 1+2 solution: blood.
Ethanol (GB679);
C sodium hydroxide (GB629) solution: 100g/L; d.
Standard disodium ethylenediaminetetraacetic acid titration solution: c(EDTA)=0.02ma1/L: Calcium indicator (NN) [Chemical name: 2-hydroxy-1-(2-hydroxy-4-iodo-J-naphthylazo)-3-naphthoic acid Preparation method: Weigh 1.0g calcium indicator and 100g sodium chloride, mix and grind finely for use, 4. 2.3*Analysis steps
Weigh 2 samples (accurate to 0.0001°C), place in a 250mL conical flask, add 15mL ethanol, 30mL water, 15mL nitric acid and heat slightly on an electric stove, keep it slightly warm until the fat carrier layer becomes transparent, cool to room temperature, filter, and rinse the filter paper continuously until the rock phosphorus test paper does not show acidity, stop rinsing, transfer the filtrate and washing solution into a 200mL volumetric flask, add water to the scale, as the test solution. Use a pipette to accurately draw 20mL of the above test solution, place in a 250mL conical flask, add water to dilute to a volume of about 100mL, add sodium hydroxide solution to adjust to pH=14, add about 0.1% of the prepared calcium indicator, and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from red to pure blue, which is the end point. 4.2.4 Expression of analysis results
The mass percentage of calcium X is given by formula (1): x,
C: Vx 0. 04008
m×200
× 100
Wu Zhong:
The actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L:
The volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in the titration, L;
The mass of the sample, g
0.04008-m-The mass of calcium in grams equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution [c(EDTA)=1.000mol/L),
4.2.5 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.2%. The arithmetic mean is taken as the calcium content, 4. 3 Determination of free acid
4.3.1 Reagents and solutions
a. Ethanol (GB 679):
b. Standard sodium hydroxide titration solution: c(NaOH) 0.05mol/L; e. Phenolic acid indicator solution: 10g/L.
4.3.2 Apparatus
5 mL microburette
4.3.3 Analysis steps
Weigh 2 samples (accurate to 0.1), add 100 mL of ethanol to a 250 mL conical flask, shake thoroughly for 5-10 minutes, then add 3-5 drops of phenolic acid indicator solution, and titrate with standard sodium hydroxide titration solution until the solution is slightly red, and the red color does not disappear within 30 seconds, which is the end point. At the same time, a blank test was performed using enzyme acetyltransferase of the same batch. 4.3.4 Expression of analytical results
The mass percentage of stearic acid, X, is given by formula (2): X,
Wherein:
c(V-V,)× 0.271
actual concentration of the standard titration solution for oxidation, m01/L; × 100
the volume of the standard titration solution of sodium hydroxide consumed in the titration, mL; V--the volume of the standard titration solution of sodium hydroxide consumed in the blank test, mL; (2)
the mass of 0.271-
industrial stearic acid equivalent to 1.00mL of the standard titration solution of sodium hydroxide (c(NaOH)=1.000mal/L), expressed in grams,
4. 4 Determination of heating loss
4.4. 1 Instruments and equipment
a. Weighing bottle: @50 mm×30 mm;
b. Electric constant temperature drying oven;
C. Dryer: Contain appropriate desiccant. 4.4.2 Analysis steps
Adjust the electric constant temperature drying oven to 105±3℃, and place the weighing bottle in the electric constant temperature drying oven to dry to constant weight. Weigh 2.5-3 g (accurate to 0.0001 g) of glass sample in a weighing bottle that has been weighed, place the weighing bottle in front of a mercury thermometer in a drying oven, open the weighing bottle cap, turn it over and put it on the side of the weighing bottle. When the temperature rises to 105±3℃, keep it for 2 hours, then cover the weighing bottle and put it into the desiccator. Weigh it after cooling for 30 minutes.
4.4.3 Expression of analysis results
The heating loss X is given by formula (3):
Where: m, the mass of the sample and weighing bottle before drying, m2
the mass of the sample and weighing bottle after drying, g: the mass of the sample, nominal.
4.5 Determination of melting point
The determination shall be carried out in accordance with the provisions of G617. The final melting point shall be the melting point. 4.6 Determination of fineness
Instruments and equipment
Test sieve (GB6003), @75mmx25mm/0.075mm; blood.
b. Soft brush: about 35mm long and 20mm wide; c. Industrial ethanol;
d: Electric constant temperature drying oven,
4.6.2 Analysis steps
Weigh sample 5 (accurate to 0.1g), place it in a 250mL flask, add 80mL of clarified industrial ethanol, shake well, pour it into the test sieve and sieve it, take another filter-proof industrial ethanol to rinse the sample in the flask and on the test sieve and sieve it, and connect the test sieve with the sieve. Place the residual sample together with the test sieve in an electric constant temperature drying oven and dry it at 85-90°C for 30 minutes. Take it out and brush it gently with a soft brush. The remaining sample on the test sieve will continue to be sieved. Finally, weigh the sieve residue that cannot be sieved (accurate to 0.0001). 4.6.3 Expression of analysis results
Fineness X, is given by formula (4):
Wu: m,—mass of sieve residue, g;
—mass of sample, more
4.7 Determination of bulk density
4.7.1 Instruments and equipment (as shown in the figure)
HG/T 2424—93
Glass funnel A;
Container B: 100±0.5cm;
Plastic plate: 30cm×3cm;
Beaker: 250mL-
4.7.2 Analysis steps
【B）
Install the instrument as shown in the figure, filter the sample thoroughly, take a sample with a volume of about 120-mL and place it in the beaker, block the outlet of the funnel with a plastic plate, then add the sample into the funnel, steadily remove the plastic plate, and let the sample fall naturally into container B. You can use a stirrer to stir the funnel carefully and slowly, and the stirring rod must not come out from the outlet of the funnel. When the container B is full of sample, use a plastic plate to block the funnel outlet to stop the sample from falling. During the above process, the container must not be moved during boiling. Put the container and the full sample on the balance and weigh (accurate to 0.1), then remove the sample and weigh the empty container again. Repeat the above operation twice and take the average value as the test result. (Calculate to four decimal places and round to three decimal places).
4.7.3 Expression of analysis results
Bulk density X, (g/cm2) Formula (5) gives: 4
Mass of container and sample, B;
Wu Zhong m
m,—mass of container, g;
V-volume of container, cm2\.
5 Inspection rules
HG/T2424-93
5.1 This product is inspected by the quality supervision department of the manufacturer. The manufacturer guarantees that the products shipped out of the factory meet the requirements of this standard and shall be accompanied by a quality certificate in a certain format.
5.2 The collection unit has the right to inspect and accept the products received in accordance with the provisions of this standard. 5.3 The products are based on the daily output as a batch.bZxz.net
5.4 The sampling number shall be determined according to Table 2 in GB/T6678. Sampling The sampling tube used for drying and cleaning is evenly hooked for sampling, and the total sampling volume shall not be less than 250. After mixing, it is divided into two bottles, one bottle is sent to the quality inspection department for inspection, and the other bottle is kept for inspection. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, it shall be re-sampled in two packaging containers for re-inspection. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.6 When the supply and demand parties have objections to the product quality, they can agree to select an arbitration unit, and the arbitration unit shall conduct arbitration inspection in accordance with the provisions of this standard.
6 Marking, packaging, transportation and storage
6.1 The product packaging bag should be painted with firm and clear markings, including the manufacturer's name, product name, product trademark, etc. 6.2 The product is packed in sealed and clean packaging such as iron barrels, wooden barrels, woven bags, etc. lined with plastic film bags. Each bag (barrel) must be accompanied by a product certificate, including the manufacturer's name, product name. Standard number, grade, index, batch number, inspection date, inspector, etc. 6.3 The product must not come into contact with acid, alkali or other corrosive substances during transportation. Pay attention to protective agents. 64 The product is stored in a cool, ventilated and dry warehouse. The storage period is 1 year. Additional instructions:
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 jurisdiction of Shanxi Chemical Research Institute. This standard was drafted by Nanjing Jinling Chemical Plant and Shanxi Chemical Research Institute. The main drafters of this standard are Wei Liangxian and Guo Yanjian. 5
People's Republic of China
Chemical Industry Standard
Calcium Stearate (Light Waist)
HG/T2424-93
Editorial Department of Swiss Chemical Industry Standard
(Chemical Industry Standardization Research Institute)
Postal Code: 100013
Indian Chemical Industry Standardization Research Institute
Copyright reserved. No printing required
Format 880 × 1230 1 / 16: Printing Sheet/16 Number of Words 10 000 First Edition in June 1993
First Printing in July 1993
Print Quantity 1 — 500
Cost 1.60 Yuan
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