Some standard content:
ICS71.060.40
Record number: 7253-2000
HG/T3607—2000
This chemical industry standard is formulated based on actual production conditions and user requirements. According to different product uses, this standard is divided into two models, Type I and Type II. Type I is mainly used as a flame retardant material, and Type II is mainly used for environmental protection.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization. The drafting units of this standard are: Tianjin Chemical Research and Design Institute of the Ministry of Chemical Industry, Guhe Magnesium Salt Factory of Jiaozhou City, Shandong Province, Shiguang of Yuncheng Salt Chemical Bureau of Shanxi Province, and Pengfei Magnesium Salt Factory of Xingtai City, Hebei Province. The main drafters of this standard are: Su Peiji, Zhang Xirong, Peng Zhenchao, and Song Kezhi. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 386
1 Scope
Chemical Industry Standard of the People's Republic of China
Magnesium hydroxide for industrial use
Magnesium hydroxide for industrial useHG/T 3607---2000
This standard specifies the requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of industrial magnesium hydroxide. This standard applies to industrial magnesium hydroxide. It is mainly used as the raw material of flame retardants, neutralization treatment of industrial acid wastewater and flue desulfurization. Molecular formula: Mg(OH)z
Relative molecular mass: 58.32 (according to the 1997 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 version of the following standards. GB/T 601—1988 Chemical reagents
Preparation of standard solutions for titration analysis (volumetric analysis) GB/T 602—1988
Chemical reagents
GB/T 603--1988
GB/T 1250—1989
GB/T 3049--1986
GB/T 3051--2000
GB/T 6678-1986
GB/T 6682-
—1992
3 Requirements
Appearance: white powder.
Chemical reagentsWww.bzxZ.net
Preparation of standard solutions for impurity determination (neqISO6353-1:1982)Preparation of preparations and products used in test methods (neqISO6353-1:1982)Expression and determination methods of limit valuesGeneral method for determination of iron content in chemical products-O-phenanthroline spectrophotometry (neqISO6685:1982)
General method for determination of chloride content in inorganic chemical products-Mercury titration (neqISO5790:1979)General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (neqISO3696:1987)Industrial magnesium hydroxide shall comply with the requirements of Table 1.
Requirements in Table 1
Magnesium oxide content
Calcium oxide content
Acid insoluble matter content
Chloride (as CI) content
Iron (Fe) content
Ignition loss
Sieve residue (75μm test sieve)
Approved by the State Administration of Petroleum and Chemical Industry on May 23, 2000 63.0
Implementation on December 1, 2000
4 Test method
HG/T3607-2000
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 products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601GB/T602 and GB/T603.
Safety Tips: The hydrochloric acid and sodium hydroxide used in the test are corrosives, so be careful when operating! 4.1 Determination of magnesium oxide content
4.1.1 Method Summary
Use triethanolamine to mask a small amount of trivalent iron, trivalent aluminum, divalent manganese and other ions. When the pH value is 10, use chrome black T as an indicator and use disodium ethylenediaminetetraacetic acid standard titration solution to titrate the calcium and magnesium contents. Subtract the calcium content from it to calculate the magnesium oxide content. 4.1.2 Reagents and Materials
4.1.2.1 Hydrochloric acid solution: 1+1.
4.1.2.2 Triethanolamine solution: 1+3.
4.1.2.3 Ammonia-ammonium chloride buffer solution: pH~10. 4.1.2.4 Silver nitrate solution: 10g/1.
4.1.2.5 Disodium ethylenediaminetetraacetic acid standard titration solution: c(EDTA) is about 0.02mol/L. 4.1.2.6 Chrome black T solid indicator: 1% (mass fraction). 4.1.3 Analysis steps
4.1.3.1 Preparation of test solution A
Weigh 7g of sample (accurate to 0.0002g), place in a 250mL beaker, moisten with a small amount of water, cover with blood, add hydrochloric acid solution to dissolve the sample, boil for 3min~5min, filter with medium-speed quantitative filter paper while hot, and wash with hot water until there is no chloride ion (check with silver nitrate solution). After cooling, transfer the filtrate and washing solution into a 500mL volumetric flask, add water to the mark, shake to obtain test solution A, which is used for the determination of magnesium oxide, calcium oxide, and iron content.
Retain the residue and filter paper for the determination of hydrochloric acid insoluble matter. 4.1.3.2 Determination
Use a pipette to transfer 25ml of test solution A, place it in a 250mL volumetric flask, add water to the mark, and shake well. Use a pipette to transfer 25ml of test solution, place it in a 250ml conical flask. Add 50mL of water, 5mL of triethanolamine solution, 10mL of buffer solution, and 0.1g of chrome black T indicator, and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from purple-red to pure blue. 4.1.4 Expression of analysis results
The magnesium oxide content (X) expressed as mass percentage is calculated according to formula (1): X, =
c × 0.040 30
m×%×250
X 100 =
806× (V;-20)g
Wherein: V.--the volume of the standard disodium ethylenediaminetetraacetic acid solution consumed in the titration, mL; V2--the volume of the standard disodium ethylenediaminetetraacetic acid solution consumed in the titration of calcium in 4.2, mL; ---the actual concentration of the standard disodium ethylenediaminetetraacetic acid solution, mol/L; (1)
m--the mass of the sample·g;
0.04030--the mass of magnesium oxide in grams equivalent to 1.00ml of the standard disodium ethylenediaminetetraacetic acid solution [c(EDTA)=1.000mol/L].
4.1.5 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 0.2%. 4.2 Determination of calcium oxide content
4.2.1 Method summary
HG/T3607—2000
Use triethanolamine to mask a small amount of trivalent iron, trivalent aluminum, divalent manganese and other ions. When the pH value is 12.5, use calcium carboxylic acid as an indicator and use ethylenediaminetetraacetic acid disodium standard titration solution to titrate calcium ions. 4.2.2 Reagents and materials
4.2.2.1 Sodium hydroxide solution: 100g/L. 4.2.2.2 Triethanolamine solution: 1+3.
4.2.2.3 Ethylenediaminetetraacetic acid disodium standard titration solution: c(EDTA) is about 0.02mol/L. 4.2.2.4 Calcium carboxylic acid [1-(2-carboxy-4-sulfonyl-1-naphthylazo)-2-hydroxy-3-carboxylic acid] solid indicator: 1% (mass fraction). Grind calcium carboxylic acid indicator and sodium ammonium chloride in a mortar in a ratio of 1:99 and store in a wide-mouth bottle with a ground stopper. 4.2.3 Analysis steps
Use a pipette to transfer 50 mL of test solution A and place it in a 250 mL conical flask. Add 30 mL of water and 5 mL of triethanolamine solution, and add sodium hydroxide solution dropwise while shaking. When the solution just becomes turbid, add 0.1 g of calcium carboxylic acid indicator and continue to add sodium hydroxide solution dropwise until the test solution changes from blue to wine red. Add 0.5 mL in excess and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from wine red to pure blue.
4.2.4 Expression of analysis results
Calcium oxide content (X2) expressed as mass percentage is calculated according to formula (2): X2 Yac×0.056 08 ×100 = 56.08Vacm×500
Wherein: V2-volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration, mL; c——actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; mass of the sample referred to in 4.1.3.1, g; m
·(2)
0.05608—mass of calcium oxide expressed in grams equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution [c(EDTA)-1.000mol/L].
4.2.5 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 0.1%. 4.3 Determination of hydrochloric acid insoluble matter content
4.3.1 Analysis steps
Transfer the filter paper and residue retained in 4.1.3.1 into a crucible with constant weight, incinerate at 850℃～900℃ until constant weight. 4.3.2 Expression of analysis results
The hydrochloric acid insoluble matter content (X3) expressed as mass percentage is calculated according to formula (3): Xg = ml=m2 ×100
Where: m—mass of crucible and insoluble matter, g; m2—mass, g;
-mass of sample referred to in 4.1.3.1, g. 4.3.3 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02%. 4.4 Determination of moisture content
4.4.1 Instruments and equipment
Weighing bottle: $50mm×30mm.
(3)
4.4.2 Analysis steps
Weigh 1g of sample (accurate to 0.0002g), place in a weighing bottle that has been dried to constant weight at 105℃～110℃, and dry at 105℃～110℃ to constant weight.
4.4.3 Expression of analysis results
HG/T 3607—2000
The moisture content (X) expressed as mass percentage shall be calculated according to formula (4): Xmi = m2 × 100
-mass of the sample and weighing bottle before drying, g; where: mr--—
ma —-
\-mass of the sample and weighing bottle after drying, g; m---mass of the sample, g.
4.4.4 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 0.1%. 4.5 Determination of chloride content
4.5.1 Summary of method
Same as Chapter 3 of GB/T3051—2
2000.
4.5.2 Reagents and materials
Same as Chapter 4 of GB/T3051-2000.
4.5.3 Instruments and equipment
Microburette: graduation value is 0.01mL or 0.02mL. (4)
4.5.4 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), place it in a 250mL beaker, add 150mL of water, cover with surface III, heat and boil for 5min~~7min, cool to room temperature, transfer to a 250ml volumetric flask, add water to the scale, and shake well. After standing for 30min, dry filter, discard the first 10mL of filtrate, transfer 50mL of filtrate and place it in a 250ml conical flask. Add 2~~3 drops of bromophenol blue indicator solution, add 1+6 nitric acid solution until it turns yellow, then add 2~3 drops in excess, add 1mL diphenylazocarbonylhydrazide indicator solution, and titrate with 0.02mol/L mercuric nitrate standard titration solution until the solution changes from yellow to purple-red. Perform a blank test at the same time.
Collect the mercury-containing waste liquid after titration and treat it according to the provisions of Appendix D of GB/T3051-2000. 4.5.5 Expression of analysis results
The chloride content (in terms of CI) expressed as mass percentage (Xs) is calculated according to formula (5): 5× 100 = 17. 73(V-Vo)c
X. =V-Vo)c×0. 035 45 ×
Wherein: V---the volume of the standard mercuric nitrate solution consumed by the titration of the test solution, mL; V--the volume of the standard mercuric nitrate solution consumed by the titration of the blank solution, mL; C--the actual concentration of the standard mercuric nitrate solution, mol/L; m--the mass of the sample, g;
Hg(NO.)2H2O]1.000mol/L) expressed in grams 0.03545.--the mass of chloride (in terms of CI) expressed in terms of 1.00mL of the standard mercuric nitrate solution (cL-).
4.5.6 Allowable difference
Take the mass of the parallel determination results. The arithmetic mean is the determination result. The absolute difference of the parallel determination results shall not exceed 0.005%. 4.6 Determination of iron content
4.6.1 Summary of method
Same as Chapter 2 of GB/T3049-1986.
4.6.2 Reagents and materials
Same as Chapter 3 of GB/T3049--1986.
4.6.3 Instruments and equipment
Spectrophotometer: with an absorption cell with a thickness of 3 cm. 390
4.6.4 Analysis steps
4.6.4.1 Drawing of working curve
HG/T 3607—2000
According to the provisions of 5.3 of GB/T3049-1986, select an absorption cell with a thickness of 3 cm and the corresponding amount of iron standard solution to draw a working curve.
4.6.4.2 Determination
Use a pipette to transfer 2.5mL of test solution A and 1ml of hydrochloric acid solution (reagent blank solution) into 100mL volumetric flasks respectively, and add water to 40mL each. The following is in accordance with the provisions of 5.4 of GB/T3049-1986, starting from "adjust the pH to 2 with ammonia water or hydrochloric acid solution, ..." to "measure its absorbance". Subtract the absorbance of the reagent blank solution from the absorbance of the test solution, and find the corresponding iron content from the working curve. 4.6.5 Expression of analysis results
The iron (Fe) content (X) expressed as mass percentage is calculated according to the formula ( 6) Calculation: X6
Where: ml-
×1000
The mass of iron found on the working curve, mg; The mass of the sample in 4.1.3.1, g. 4.6.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.005%. 4.7 Determination of loss on ignition
(6)
4.7.1 Summary of method
At 550℃~600℃, the magnesium hydroxide in the sample loses water to become magnesium oxide and loses free water at the same time. The loss on ignition is determined based on the reduced mass of the sample.
4.7.2 Analysis steps
Weigh 1g of sample (accurate to 0.0002g), place it in a porcelain crucible with constant weight, and ignite it at 550℃~~600℃ until constant weight. 4.7.3 Expression of analysis results
The ignition loss (X,) expressed as mass percentage shall be calculated according to formula (7): X = ml=m2 ×100
Wherein: ml-
The mass of the sample and the flask before ignition, m;
The mass of the sample and the flask after ignition, g;
The mass of the sample, g.
4.7.4 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 0.1%. 4.8 Determination of sieve residue
4.8.1 Summary of method
The sample shall be sieved through a standard sieve, and the product sieve residue shall be determined according to the mass of the sample on the test sieve. 4.8.2 Instruments and equipment
4.8.2.1 Test sieve: R403 series, Φ200mm×50mm/75μm. 4.8.2.2 Soft brush: The length of the brush is about 3 cm and the width of the brush is about 5 cm. (7)
4.8.3 Analysis steps
Weigh about 10 g of sample (accurate to 0.01 g), transfer it to the test sieve, and gently brush the sample with a soft brush to make the powder pass through. Finally, place a piece of black paper under the sieve and brush the sieve until no trace is left on the black paper. Transfer the sieve residue to a surface dish of known mass and weigh it (accurate to 0.000 2 g).
4.8.4 Expression of analysis results
HG/T 3607---2000
The sieve residue (X.) expressed as a mass percentage is calculated according to formula (8): Xs = m2=mi ×100
Where: ml--mass of surface blood, g; m2--mass of surface blood and sieve residue, gm\mass of sample, g.
4.8.5 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 be greater than 0.1%. 5 Inspection rules
5.1 All items specified in this standard are routine test items. 5.2 Each batch of products shall not exceed 50t.
(8)
5.3 Determine the number of sampling units in accordance with the provisions of (GB/T6678. 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 a sample. After mixing the collected samples, reduce them to not less than 500g by the quartering method, and pack them into two clean and dry wide-mouth bottles with stoppers and seal them. Attach labels to the bottles, indicating: manufacturer name, product name, model, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other is kept for three months for future reference.
5.4 Industrial magnesium hydroxide should be inspected by the quality supervision and inspection department of the manufacturer in accordance with The manufacturer shall ensure that all industrial magnesium hydroxide shipped out of the factory meets the requirements of this standard. 5.5 The user has the right to inspect and accept the industrial magnesium hydroxide products received in accordance with the provisions of this standard, and the acceptance time shall be within one month after the arrival of the goods.
5.6 If any indicator of the inspection result does not meet the requirements of this standard, re-samples shall be taken from twice the amount of packaging for re-inspection. If even one indicator of the re-inspection result does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.7 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the standard . 6 Marking and labeling
6.1 The packaging of industrial magnesium hydroxide should have firm and clear markings, including: manufacturer name, address, product name, trademark, model, net content, batch number or production date, and this standard number. 6.2 Each batch of magnesium hydroxide products leaving the factory should be accompanied by a quality certificate, including: manufacturer name, address, product name, trademark, model, net content, batch number or production date, proof that the product quality complies with this standard and this standard number. 7 Packaging, transportation, storage
7.1 The inner packaging of industrial magnesium hydroxide shall be made of polyethylene plastic film bags with a thickness of not less than 0.05mm. The outer packaging is made of plastic woven bags, and its performance and inspection methods shall comply with relevant regulations. The net content of each bag is 25kg. The inner bag is tied twice with nylon rope, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the bag edge, and sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the bag edge. The stitches are neat and the stitch length is uniform. There is no leakage or skipping.
7.2 Industrial magnesium hydroxide should be covered during transportation to prevent rain and moisture. 7.3 Industrial magnesium hydroxide should be stored in a cool and dry place to prevent rain and moisture. 392
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