Some standard content:
Record number: 7250-2000
HG/T2959--2000
This standard is a text conversion of the chemical industry standard HG/T2959-1988 "Industrial Hydrated Basic Magnesium Carbonate". This standard will replace HG/T2959-1988 from the date of implementation. This standard is proposed by the Policy and Regulations Department of the State Bureau of Petroleum and Chemical Industry. This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization. The drafting unit of this standard: Tianjin Chemical Research and Design Institute. The main drafters of this standard: Yao Jinjuan, Shi Jie. This standard was first issued as a national standard in 1979, revised for the first time in 1988, and converted to HG/T2959--1988 in 1997
This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 882
1 Scope
Chemical Industry Standard of the People's Republic of China
Industrial Hydrated Basic Magnesium Carbonate
Hydrated basic magnesium carbonate for industrial useHG/T 2959--2000
Replaces HG/T29591988
This standard specifies the requirements, test methods, inspection rules, and marking, labeling, packaging, transportation and storage of industrial hydrated basic magnesium carbonate. This standard applies to industrial hydrated basic magnesium carbonate made from dolomite, brine and sodium carbonate. This product is mainly used in industries such as rubber, thermal insulation materials, plastics and pigments as a filler and reinforcing agent. Molecular formula: αMgCO3·yMg(OH)2·zH,O2 Reference Standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards will be revised. All parties using this standard should explore the possibility of using the latest version of the following standards. GB191-1990 Pictorial markings for packaging, storage and transportation
GB/T601-1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T602-1988 Preparation of standard solutions for determination of impurities in chemical reagents (neqISO6353-1:1982) GB/T603-1988 Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982) GB/T1250-1989 Limit values Expression and determination methods GB/T3049--1986 General method for determination of iron content in chemical products O-phenanthroline spectrophotometry (neqISO66851982) GB/T3051-2000 General method for determination of chloride content in inorganic chemical products Mercury titration (neqISO5790:1979) GB/T6678-1986 General principles for sampling of chemical products Specifications and test methods for water in analytical laboratories (negISO3696:1987) GB/T 6682--1992
3 Requirements
3.1 Appearance: White light powder.
3.2 Industrial hydrated basic magnesium carbonate shall meet the requirements of Table 1. Approved by the State Administration of Petroleum and Chemical Industry on May 23, 2000, and implemented on December 1, 2000
Water content, %
Hydrochloric acid insoluble matter, %
Calcium oxide (Ca()) content, %
Magnesium oxide (MgO) content, %
Loss on ignition, %
Chloride (as Cl) content, %
Iron (Fe) content, %
Manganese (Mn) content, %
Sulfate (as SO4) content, %
Sieve residue: 150μm, %
75 μm,%
Bulk density, g/mL
HG/T2959—2000
Requirements in Table 1
Superior products
Note: The moisture content of superior products refers to the value at the time of packaging, and the moisture content should be marked in a conspicuous place. Test method
First-class products
Qualified products
Greater than 52.0
The reagents and water used in this standard refer to analytical pure reagents and grade 3 water specified in GB/T6682 unless otherwise specified. The standard titration solutions, impurity standard solutions, preparations and products used in the test refer to those specified in GB/T601 and GB /T602, GB/T603.
Safety Tips: The strong acids and alkalis used in this standard are corrosive. Users should be careful when handling them. If they splash on the skin, rinse immediately with plenty of water. In severe cases, seek medical treatment immediately!
4.1 Determination of moisture content
4.1.1 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place it in a 40mm×25mm weighing bottle with constant weight, and move it to a constant temperature drying oven at 105℃～110℃ to dry it to constant weight.
4.1.2 Expression of analysis results
The moisture content (X,) expressed as mass percentage is calculated according to formula (1): mi -
Where: mt-
The mass of the sample and weighing bottle before drying, g; -The mass of the sample and weighing bottle after drying, g; The mass of one sample, 8.
4.1.3 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 0.05%. 4.2 Determination of hydrochloric acid insoluble matter content
4.2.1 Reagents and materials
4.2.1.1 Hydrochloric acid solution: 1+1.
4.2.1.2 Silver nitrate solution: 10g/L.
4.2.2 Instruments and equipment
HG/T 2959—2000
High temperature furnace: can control the temperature at 850℃~900℃. 4.2.3 Analysis steps
Weigh about 5g of sample (accurate to 0.0002g), place it in a 250mL beaker, add a small amount of water to moisten it, cover it with a watch glass, slowly add hydrochloric acid solution to dissolve the sample (about 25mL), boil for 3min~~5min, filter it with medium-speed quantitative filter paper while it is hot, wash the precipitate with hot water until the filtrate does not contain chloride ions (check with silver nitrate solution). Transfer the filter paper and insoluble matter to a constant-weight porcelain crucible, transfer them to a high-temperature furnace after ashing, and burn them at 850℃~~900℃ to constant weight. Transfer the filtrate and washing solution to a 250mL volumetric flask, add water to the scale, and shake well. This solution is test solution A. For the determination of calcium oxide, magnesium oxide, iron and sulfate content. 4.2.4 Expression of analysis results
The hydrochloric acid insoluble matter content (X,) expressed as a mass percentage is calculated according to formula (2): Xz = ml=m2×100
Wherein: ml
Mass of crucible and hydrochloric acid insoluble matter after calcination, g; mass of crucible, g;
mMass of sample, g.
4.2.5 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 0.02%. 4.3 Determination of calcium oxide content
4.3.1 Summary of method
A small amount of Fe3+, A13+, Mn2+ ions are masked with triethanolamine, and the sodium salt of calcium reagent carboxylate is used as an indicator. The pH value is adjusted to be greater than 12, and titrated with a standard titration solution of disodium ethylenediaminetetraacetic acid. 4.3.2 Reagents and materials
4.3.2.1 Sodium hydroxide solution: 100 g/L. 4.3.2.2 Triethanolamine solution: 1 + 3.
4.3.2.3 Ethylenediaminetetraacetic acid disodium standard titration solution: c (EDTA) is about 0.02 mol/L. 4.3.2.4 Calcium reagent carboxylate sodium salt indicator. Grind calcium reagent carboxylate sodium salt and sodium chloride in a mortar in a ratio of 1 + 99, mix well and store in a wide-mouth bottle with a ground stopper. 4.3.3 Analysis steps
Weigh 50.00mL of test solution A and place it in a 250mL conical flask. Add 40mL of water and 5mL of triethanolamine solution. Add sodium hydroxide solution dropwise while shaking. When the test solution becomes turbid, add a small amount of calcium reagent sodium carboxylate mixed indicator. Continue to add sodium hydroxide solution dropwise until the test solution changes from blue to wine red. Add 0.5mL in excess and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution becomes pure blue. 4.3.4 Expression of analysis results
Calcium oxide (CaO) content (X) expressed as mass percentage is calculated according to formula (3): Xx = Ve×0.056 08 ×100 = 2m×250
28.04 X Vc
Wherein: V—volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration, mL; c—actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; m—mass of the sample weighed in 4.2.3, g; · (3)
0.05608--The mass of calcium oxide in grams equivalent to 1.00mL of disodium ethylenediaminetetraacetic acid standard titration solution Ec(EDTA)=1.000mol/L.
4.3.5 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 0.02%. 4.4 Determination of magnesium oxide content
4.4.1 Summary of method
HG/T 2959--2000
A small amount of Fe3+, A13+, Mn2+ ions are masked with triethanolamine. Under the condition of pH 10, chrome black T is used as an indicator, and the total amount of calcium and magnesium is titrated with disodium ethylenediaminetetraacetic acid standard titration solution, from which the calcium content is subtracted. 4.4.2 Reagents and materials
4.4.2.1 Triethanolamine solution: 1+3.
4.4.2.2 Ammonia-ammonium chloride buffer solution A: pH=10. 4.4.2.3 Ethylenediaminetetraacetic acid disodium standard titration solution: c(EDTA) is about 0.02mol/1. 4.4.2.4 Eriochrome black T indicator.
Grind Eriochrome black T and sodium chloride in a mortar in a ratio of 1+99, mix well, and place in a wide-mouth bottle. 4.4.3 Analysis steps
Pipette 25.00mL of test solution A, place in a 250mL volumetric flask, add water to the mark, and shake well. Pipette 25.00mL and place in a conical flask, add 50mL of water, 5mL of triethanolamine solution, 10mL of buffer solution and a small amount of Eriochrome black T indicator, and titrate with ethylenediaminetetraacetic acid disodium standard titration solution until the solution changes from purple-red to pure blue. 4.4.4 Expression of analysis results
The magnesium oxide (MgO) content (X) expressed as mass percentage is calculated according to formula (4): XA
c X 0. 040 30
250×250
Wherein: V-volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration, mL; V
(4)
-volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration of calcium in 4.3, mL; c---actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; m-
-mass of the sample weighed in 4.2.3, g; -mass of magnesium oxide in grams equivalent to 1.00 mL disodium ethylenediaminetetraacetic acid standard titration solution [c(EDTA)=1.000mol/L].
4.4.5 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 0.12%. 4.5 Loss on ignition
4.5.1 Summary of method
At 850℃～~900℃, the sample is completely decomposed into magnesium oxide and releases carbon dioxide and water, and its loss is measured. 4.5.2 Instruments and equipment
High temperature furnace: capable of controlling the temperature at 850℃～900℃. 4.5.3 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place it in porcelain that has been constant weight at 850℃～900℃, and ignite it in a high temperature furnace at 850℃~～900℃ to constant weight.
4.5.4 Expression of analysis results
The ignition loss (X,) expressed as a mass percentage is calculated according to formula (5): Xs=m=m2×100-X
Wherein: m
The mass of the sample and the crucible before ignition, g;
The mass of the sample and the crucible after ignition, g;
The mass of the sample, g;
X4.1 The measured moisture,%.
4.5.5 Allowable differencebZxz.net
(5)
HG/T2959—2000
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the parallel determination results shall not exceed 0.05%. 4.6 Determination of chloride content
4.6.1 Summary of the method
According to Chapter 3 of GB/T3051—2000.
4.6.2 Reagents and materials
According to Chapter 4 of GB/T3051-2000.
4.6.3 Analysis steps
Weigh about 5g of sample (accurate to 0.01g), place in a conical flask, add a small amount of water to moisten, slowly add 1+1 nitric acid solution until the sample is completely dissolved, add 2 to 3 drops of bromophenol blue indicator solution, if the test solution is yellow, then add sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 2 to 3 drops in excess. If the test solution is blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 2 to 3 drops in excess. Add 1ml. diphenylazocarbonylhydrazide indicator solution, and titrate with standard mercuric nitrate titration solution until the solution changes from yellow to purple-red. Perform a blank test at the same time.
4.6.4 Expression of analysis results
The chloride content (in terms of CI) expressed as mass percentage (X.) is calculated according to formula (6): (VV.)c×0.035 45×100=
X. =-
Wherein: V is the volume of the standard titration solution of mercuric nitrate consumed in titration, mL; V. is the volume of the standard titration solution of mercuric nitrate consumed in blank test, mL; the actual concentration of the standard titration solution of mercuric nitrate, mol/L0.035 45-
. 3.545(V- Vo)c
The mass of chlorine in grams equivalent to 1.00mL of standard mercuric nitrate titration solution (cL(Hg(NO,)z=1.000mol/L).
4.6.5 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 0.02%. 4.7 Determination of sulfate content
4.7.1 Summary of the method
In a dilute hydrochloric acid medium, sulfate ions are precipitated with barium chloride. Compare its turbidity with that of barium sulfate standard suspension. 4.7.2 Reagents and materials
4.7.2.1 Hydrochloric acid solution: 1+1.
4.7.2.2 Ammonia solution: 1+4.
4.7.2.3 Barium chloride solution: 100g/L.
4.7.2.4 Sulfate standard solution: 1mL solution contains 0.1mgSO4. 4.7.3 Analysis steps
Pipette the amount of test solution A and sulfate standard solution specified in Table 2 and place them in 50 mL colorimetric tube, adjust the test solution to neutrality with ammonia water (check with pH test paper), add 10mL water, 1mL hydrochloric acid solution and 2mL barium chloride solution, add water to the scale, shake the hook, place in a 40℃～50℃ water bath, and compare with the standard after 10 minutes. The turbidity shall not be darker than the standard. Table 2 Amount of test solution and standard solution pipetted
Test solution A/ml
Sulfate standard solution/mL
4.8 Determination of iron content
4.8.1 Summary of method||tt| |Same as Chapter 2 of GB/T3049-1986.
Superior products
First-class products
Qualified products
4.8.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986.
4.8.3 Instruments and equipment
Same as Chapter 4 of GB/T3049-1986.
4.8.4 Analysis steps
4.8.4.1 Drawing of working curve
HG/T 2959—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, and draw a working curve.
4.8.4.2 Preparation of blank test solution
Measure 25mL of hydrochloric acid solution in a 250mL volumetric flask and add water to the scale. 4.8.4.3 Determination
Pipette 10.00mL (or 5.00mL) of test solution A and blank solution, place them in 100mL volumetric flasks respectively, and add about 40mL of water to each. The following operations are in accordance with the provisions of 5.4 of GB/T3049--1986, starting from ".....If necessary, add water to 60mL" to "measure its absorbance".
Subtract the absorbance of the reagent blank solution from the absorbance of the test solution, and find out the iron content in the test solution from the working curve. 4.8.5 Expression of analysis results
The iron (Fe) content (X,) expressed as mass percentage is calculated according to formula (7): o ×100 = 0.1m
X,=mx1000
wherein mj-the mass of iron in the test solution, mg; mo-the mass of iron in the blank solution, mg; m is the mass of the sample removed from the test solution A + g. 4.8.6 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 0.003%. 4.9 Determination of manganese content
4.9.1 Method Summary
In a strong acidic medium in the presence of phosphoric acid, potassium periodate is used to oxidize the divalent manganese ions in the test solution into purple-red permanganate ions, and its absorbance is measured by a spectrophotometer at the maximum absorption wavelength (525nm). 4.9.2 Reagents and Materials
The water used in this test should not contain reducing substances. 4.9.2.1 Potassium periodate.
4.9.2.2 Phosphoric acid solution: 1+1.
4.9.2.3 Nitric acid solution: 1+1.
4.9.2.4 Ammonia solution: 2+3.
4.9.2.5 Manganese standard solution: 1mL solution contains 0.01mgMn. Use a pipette to transfer 25mL of the standard solution prepared according to GB/T602, place it in a 250mL volumetric flask, dilute it to the mark with water, and shake it well. The dilution solution should be prepared before use.
4.9.3 Instruments and equipment
Spectrophotometer: with an absorption cell of 3 cm thickness. 4.9.4 Analysis steps
4.9.4.1 Working curve drawing
Use a pipette to transfer: 0mL, 5.00mL, 10.00mL, 15.00mL, 20.00ml. and 25.00mL of manganese standard solution, respectively, into 250mL beakers, add 40mL of water, 1.5mL of nitric acid solution, 10mL of phosphoric acid solution and 0.5g of potassium periodate, cover with surface 888
HG/T2959—2000
blood, heat and boil until the purple-red color of permanganate appears, then gently boil for 3 minutes, cool and transfer all into a 100mL volumetric flask, add water to the scale, and shake well.
At a wavelength of 525nm, use a 3cm absorption cell and water as a reference, adjust the absorbance of the spectrophotometer to zero, and measure its absorbance. Use the manganese content as the horizontal axis and the corresponding absorbance as the vertical axis to draw a working curve. 4.9.4.2 Preparation of blank test solution
Measure 5mL of nitric acid solution, place it in a beaker, adjust the pH value to 7 with ammonia solution (check with pH test paper), and then add 1.5ml of nitric acid solution.
4.9.4.3 Determination
Weigh about 5g of the sample (accurate to 0.01g), place it in a beaker, add a small amount of water to moisten it, add 20mL of nitric acid solution to dissolve the sample, heat the test solution to boiling, filter it with medium-speed quantitative filter paper while it is hot, collect the filtrate and washing liquid in a 250mL beaker together, and at the same time as the blank test solution, perform the following operations as described in 4.9.4.1, starting from "add 10mL of phosphoric acid..." until its absorbance is measured. Subtract the absorbance of the blank test solution from the absorbance of the sample, and find the manganese content in the sample from the working curve. 4.9.5 Expression of analytical results
The manganese (Mn) content (X:) expressed as mass percentage is calculated according to formula (8): ×100 = 0. 1 ml
X:=mx1000
Where: ml——mass of manganese in the test solution, mg; mass of a sample, g.
4.9.6 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 0.004%. 4.10 Determination of sieve residue
4.10.1 Instruments and equipment
4.10.1.1 Test sieve: R40/3 series Φ200mmX50mm/0.075mm and $200mmX50mm/0.150mm. 4.10.1.2 Brush : No. 1 wool brush.
4.10.2 Analysis steps
. (8)
Weigh about 10g of sample (accurate to 0.01g), transfer it into the test sieve once or several times, mix it with water, shake the sieve while gently rinsing it with tap water until the sample no longer passes through, brush it lightly on the sieve with a brush, rinse the brush and sieve with water until the rinse water does not contain the sample, and then rinse the test sieve with 95% ethanol, transfer the sieve together with the sieve residue into a constant temperature drying oven, dry it at (105±5)℃, transfer the sieve residue to a surface III or sulfuric acid paper of known mass and weigh it (accurate to 0.0002 g), 4.10.3 Expression of analysis results
The sieve residue (X.) expressed as a mass percentage is calculated according to formula (9): X. =㎡×100
Wherein: ml—-mass of sieve residue, g;
m—-mass of sample, g.
4.10.4 Allowable difference
(9)
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: 0.003% for 150μm test sieve; 0.04% for 75μm test sieve.
4.11 Determination of bulk density
4.11 .1 Instruments and equipment
Bulk density tester, as shown in Figure 1. The funnel is fixed on the bracket, and the measuring cylinder is located below the center line of the funnel, with a distance of about 30mm. 889
4.11.2 Analysis steps
HG/T2959--2000
1-500ml (or 250mIL) measuring cylinder; 2- bracket; 3- funnel Figure 1 Bulk density tester
Within 1 minute, let the sample fall freely from the funnel into the measuring cylinder of known mass and volume. The sample should be higher than the wall of the measuring cylinder. Use a ruler to scrape off the sample that is higher than the upper end of the measuring cylinder and weigh it (accurate to 0.01g). 4.11.3 Expression of analysis results
Bulk density (Xio) in g/mL is calculated according to formula (10): mass of the sample, g;
where: m-
volume of the measuring cylinder, mL.
4.11.4 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 0.02g/mL. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 The mass of each batch of products shall not exceed 60t. (10)
5.3 Determine the number of sampling units according to GB/T6678. When sampling, the sampler should be inserted obliquely from the top of the packaging bag to 3/4 of the depth of the material layer for sampling. After mixing the collected samples, divide them into quarters to not less than 500g and pack them in two clean, dry wide-mouth bottles with stoppers. The density of the bottles is marked with labels 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 is kept for three months for future reference. 5.4 Industrial hydrated basic magnesium carbonate shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard; the manufacturer shall ensure that all industrial hydrated basic magnesium carbonate shipped from the factory meets the requirements of this standard. 5.5 The user has the right to inspect and accept the industrial hydrated basic magnesium carbonate received in accordance with the provisions of this standard, and the inspection and acceptance shall be carried out within two months from the date of arrival.
5.6 If any of the indicators in the inspection results do not meet the requirements of this standard, samples shall be taken from twice the amount of packaging bags for re-inspection. If even one of the indicators in the re-inspection results 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 hydrated basic magnesium carbonate shall be firmly and clearly marked, including: manufacturer name, address, product name, trademark, grade, net content, batch number or production date, this standard number and the "wet-afraid" mark specified in GB191. 890
HG/T2959—2000
6.2 Each batch of industrial hydrated basic magnesium carbonate shipped shall be accompanied by a quality certificate, including: manufacturer name, address, product name, trademark, grade, net content, batch number or production date, proof that the product quality meets this standard and this standard number. 7 Packaging, transportation and storage
7.1 Industrial hydrated basic magnesium carbonate adopts two packaging methods. 7.1.1 Plastic woven bag packaging: The inner packaging adopts polyethylene plastic film bags with a thickness of not less than 0.03mm; the outer packaging adopts plastic woven bags, and its performance and inspection methods shall comply with relevant regulations. The net content of each bag is 50kg, 40kg or 25kg. 7.1.2 Laminated bag packaging: Its performance and inspection methods shall comply with relevant regulations. The net content of each bag is 50kg, 40kg or 25kg. 7.2 When industrial hydrated basic magnesium carbonate is packaged in plastic woven bags, the inner bag is tied with vinyl rope or other ropes of equivalent quality, or sealed with other equivalent methods; the outer bag is sewn with vinyl thread or other threads of equivalent quality. When using laminated bag packaging, the edge should be folded 30mm away from the bag edge, and the edge should be sewn with vinyl thread or other threads 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.
7.3 Industrial hydrated basic magnesium carbonate should be covered during transportation to prevent it from being exposed to the sun, rain, and moisture. It must not be transported together with acids. 7.4 Industrial hydrated basic magnesium carbonate should be stored in a cool and dry place, away from sunlight, rain and moisture, and should not be stored together with acid.
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