Some standard content:
GB17513—1998
This standard is based on the investigation of domestic and foreign conditions, combined with the characteristics of production, scientific research and trade of realgar and orpiment mines in my country, and in accordance with CB/T12707—1991 "Guidelines for Quality Grading of Industrial Products", the products of realgar and orpiment mines are graded according to their quality. The determination of the test method of this standard is based on the results of the semi-quantitative spectrum, differential thermal and total analysis of the samples, and the comprehensive conditional tests are carried out on the sample collection and preparation methods, the analysis methods of iodine trioxide and water content. The masking agent is used to mask the impurity determination high content, which simplifies the analysis process and improves the accuracy and precision of the method. The test methods of iodine trioxide and water content are all classical methods, which are accurate, reliable and highly operable.
This standard replaces [IG/T 2275.~2275.4—:t992] from the date of implementation. This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Chemical Raw Materials and Minerals Standardization Technical Committee of the Ministry of Chemical Industry. The drafting units of this standard are Lianyungang Design and Research Institute of the Ministry of Chemical Industry and Hunan Realgar Mine. The main drafters of this standard are Zhao Zhiquan, Luo Lin, Yu Ruyun, Huang Xiaoshi and Yang Rubin. Lianyungang Design and Research Institute of the Ministry of Chemical Industry is entrusted with the interpretation of this standard. 1
National Standard of the People's Republic of China
Realgar and orpiment
GB 17513--1998
This standard specifies the requirements, sampling and sample preparation, test methods, inspection rules, marking, packaging, transportation and storage and safety of realgar and orpiment products.
This standard applies to realgar and orpiment products used in chemical, metallurgical, pharmaceutical, military and other departments. Referenced 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 valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest version of the following standards. GB/T 601--1988
GB/T 602—1988
G3/T 603--1988
GB/T 1250—1989
GB/T 6003- 1985
GB/T 6678
GB/T 6682--1992
G13/T 8547—1988
3 Requirements
3.1 Appearance
Chemical reagents
Chemical reagents
Chemical reagents
Preparation of standard bath solution for titration analysis (volume analysis) Preparation of standard wave for impurity determination (negISO6853-1:1982) Preparation of preparations and products used in test methods (negIS()6853-1:1982) Methods of expressing and determining limit values Test sieves
Chemical product sampling plan
Specifications and test methods for water in analytical experiments (eqvISO3696:1987) Composite plastic woven bags
Realgar lump: dark red or orange red.
Realgar concentrate; orange yellow.
Orpiment lump: lemon yellow or bright purple
Orpiment concentrate; lemon yellow.
3.2 The technical indicators of realgar lump ore products shall meet the requirements of Table 1. Approved by the State Administration of Quality and Technical Supervision on October 19, 1998 and implemented on April 1, 1999
Realgar (As2S2) content
Arsenic trioxide (As:0)) containing
Water (H0)
Except for water, the content of each component is calculated on a basis basis
GB 17513--1998
Technical indicators of realgar lump ore products
Superior products
The indicators of arsenic trioxide are the requirements for raw materials for medicine, and no requirements are made for other uses. The technical indicators of Yaohuang concentrate products shall meet the requirements of Table 2.3
Table 2 Technical indicators of realgar concentrate products
Superior products
Regal (As2S,) content
As () content
Water (H)
Except for water, the contents of each component are calculated on a dry basis. 90.0
The indicator of realgar concentrate is the requirement for raw materials for medicine, and no adjustment is made for other purposes. 3.4 The technical indicators of realgar concentrate products shall meet the requirements of Table 3. Table 3 Technical indicators of orpiment lump ore products
Orpiment (A525,) content
Moisture (H.2O) content
Superior product
Note: Except for moisture, the content of each component is calculated on a dry basis. 3.5 Technical indicators of orpiment concentrate products shall comply with the requirements of Table 4 Table 1 Technical indicators of orpiment concentrate products
Orpiment (As,S,) content
Moisture (H.2O) content
Superior product
Note: Except for moisture, the content of each component is calculated on a dry basis. First-class product
Qualified product
Qualified product
Qualified product
4 Sampling and sample preparation
4.1 Sampling
4.1.1 Number of samples
GB 17513—1998
4.1.1.1 The total amount of samples of blocky realgar ore and orpiment ore shall not be less than one thousandth of the batch, and the amount of the sample shall not be less than 250g. 4.1.1.2 The total amount of samples of flotation concentrate products shall not be less than one ten-thousandth of the batch, and the amount of the sample shall not be less than 50g. 4.1.1.3 The number of boxes and bags selected shall comply with the provisions of 6.6.1 of GB/T6678-1998. The total number of boxes and bags less than 500 shall be determined in accordance with the provisions of Table 5. The total number of boxes and bags greater than 500 shall be determined in accordance with the provisions of 3×N\ (N is the total number of bags of each batch of products). Table 5 The number of boxes and bags selected
Total number of boxes and bags (N)
50 -~64
65-~81
82~-[0]
102--125
126~151
152--181
4.1.2 Operation method
4.1.2.1 Ore pile sampling
Sampling box, number of bags (n)
Total number of bags (N)
182-216
217-254
297~-343
344--39
395--150
451-512
Sampling box, number of bags (n)
Sampling is done at 0.1 m from the surface. The sampling point should be no less than 0.1mm from each side (or bottom) and the incremental samples taken at each point should be similar.
A grid is laid out on the ore pile with a line spacing of 1m on the plane. A sampling shovel is used to take incremental samples at each intersection (as shown in Figure 1). The amount of incremental samples taken and the total amount of samples should comply with the provisions of 4.1.1.1 or 4.1.1.2. 4.1.2.2 Sampling of packaging boxes
N boxes are randomly selected according to the provisions of 4.1.1.3. Points are arranged in each box according to Figure 2. Two incremental samples are taken with a sampling shovel. The amount of incremental samples and the total amount of samples should comply with the provisions of 4.1.1.1.
阁】Schematic diagram of sampling points for ore piles
Figure 2 Schematic diagram of sampling points for wooden boxes
4.1.2.3 Sampling of packaging bags
According to the provisions of 4.1.1.3, randomly capture n bags, and use a sampling shovel (block code) or a sampling probe (concentrate) to collect two additional samples in each connection. The amount of additional samples and the total amount of samples should comply with the provisions of 4.1.1.1 or 4.1.1.2. 4.2 Sample preparation
4.2.1 Combine, crush, sieve and mix the original samples taken from the same batch. The processing process is carried out step by step according to formula (1). Q Kd
Where: Q is the minimum reliable mass of the sample, kg; d is the maximum particle size of the sample, mm; - reduction coefficient, take 0.2.
（1）
4.2.2 The sample is crushed and reduced to about 1 kg according to the provisions of 4.2.1, and ground until it can pass through the 2 μm standard sieve. Take out about 500 g of the sample and divide it into two clean and dry brown ground-mouth bottles or plastic bags. After sealing, label them and indicate the sample name, number, batch number, production unit, sampling date, location and sampler. One bottle is used as a laboratory sample for moisture determination, and the other bottle is used as a preparatory sample. The preparatory sample is retained for two months.
4.2.3 The remaining sample is further ground and reduced to about 100 g and can pass through the 150 μm standard sieve. This sample is the final sample. Note: If the sample has a high moisture content and is inconvenient to prepare, it can be pre-dried at 80°C. 4.2.4. Mix the final sample thoroughly and pack it in equal amounts into two clean and dry brown bottles or plastic bags. After resealing, label them with the sample name, batch number, production unit, sampling period, location and sampler. Store in a dark place. One bottle is used as a laboratory sample for determining the main content and arsenic trinitride, and one bottle is used as a preparatory sample. The preparatory sample is kept for three months. 5. Test method
The water composition used in this standard meets the specifications of grade 3 water in GB/T6682. The listed reagents, unless otherwise specified, refer to analytical pure reagents. The standard solutions, residual standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB/T601, GIB/T602 and GB/T603 unless otherwise specified. 5.1 Determination of Arsenic Content Iodine Method (Arsenic Method)
5.1.1 Summary of Method
After the sample is decomposed with nitric acid saturated with potassium nitrate, the nitric acid is driven out with sulfuric acid. In a strong acid solution, the pentavalent arsenic is reduced to divalent arsenic with potassium iodide. The solution is boiled to remove iodine, and the interfering arsenic is masked with sodium tartrate. Then, in a slightly alkaline solution, the arsenic is titrated with an iodine standard titration. As0 +I +0 -As0, +21 +2H
5. 1.2 Reagents and solutions
5. 1.2. 1
5. 1. 2. 2
5. 1. 2. 4
5. 1. 2. 5
5. 1. 2. 6
5. 1. 2. 7
5. 1. 2. 8
Sodium bicarbonate
Potassium iodide.
Sodium tartrate solution: 200g/L.
Sodium hydroxide solution: 200g/L.
Sulfuric acid (p: 1.84 g/ml.) solution: 1-1
Sulfuric acid solution: 1+10.
Boric acid solution saturated with potassium fluoride: Weigh about 100g potassium chlorate and dissolve it in 1,000ml nitric acid (p:1.40g/mL). Starch solution: 5g/L. Weigh 0.5g soluble starch and add a small amount of water to make it into a slurry. After it is cooked, pour it into 100ml boiling water while stirring. If it is turbid, heat it until it is clear. Let it cool and then use it (prepare it when needed). 5.1.2.9
Sodium thiosulfate (Na25,0,5H2O) solution: 2.5 g/L, weigh 2.5 g of sodium thiosulfate in hot distilled water that has just been boiled and cooled, add 0.1 ml of sodium carbonate, dilute to 1 000 ml with the same water, shake, and store in a brown reagent bottle. 5.1.2.10 Carbon standard titration solution c: (1/21,)-=0.1 ml01/1. Prepare and calibrate according to 4.9 of G13/T 601-1988. 5.1.2.11 Phenolic acid indicator solution: 5 g/L ethanol solution. 5.1.3 Sample
The sample is dried at (80±3)°C for more than 2 h and placed in a desiccator to cool to room temperature. 5.1.4 Analysis steps
Use the difference method to weigh 0.1 ~ 0.2 g or sample, accurate to 0.0002 g, place in a 250 mL chain bottle, moisten with a small amount of water, add 10 mL of potassium chlorate saturated nitric acid solution (5.1.2.7), wait for the reaction to subside, and heat at low temperature until it is completely decomposed. Add about 8 mL of sulfuric acid solution (5.1.2.5), heat until thick white smoke of sulfur trioxide is emitted, remove and cool, rinse the bottle wall with a small amount of water, and continue to heat until white smoke is emitted. Cool, rinse the bottle with water and dilute to about 50 mL, heat to dissolve soluble salts, add 1 g of potassium iodide (5.1.2.2), shake, and heat to boiling. Dilute to 100 mL with hot water, continue to heat and boil to expel most of the free iodine, and the solution turns light yellow. Cool rapidly, add 23 ml of sodium tartrate solution (5.1.2.3), dilute to 100 ml with water, add 5 ml of powder solution (5.1.2.8), add sodium thiosulfate solution (5.1.2.9) until the blue-purple color just disappears. Add two drops of phenol indicator solution (5.1.2.11). Neutralize with sodium hydroxide solution (5.1.2.4) until the solution turns red, add sulfuric acid solution (5.1.2.6) until the red color just disappears, add one more drop, and cool. Add 3 g of sodium bicarbonate (5.1.2.1), immediately titrate with iodine standard titration solution (5.1.2.10) until the purple color is reached, which is the end point. Perform a blank test at the same time as the sample determination.
5.1.5 Expression of analysis results
GB 17513-1998
5.1.5.1 The arsenic (As) content (Xf) expressed as mass percentage is calculated according to formula (2): Xf - c(V - Ve) × 0.03746 × 100m
Wherein: c-actual liquid concentration of iodine standard titration solution, mal/l.; volume of iodine standard titration solution consumed by the sample, ml. V-volume of iodine standard titration solution consumed in the blank test, L; m-mass of the sample, g;
0.03746
is titrated with 1.00 ml of iodine standard titration solution [c(1/21,)=1.000 mol/1.7 equivalent, the mass of arsenic expressed in points, 5.1.5.2 The content of realgar (As2S) expressed in mass percentage (X2) is calculated according to formula (3): X - X1 X 1. 427 9
Wherein: X}--mass percentage of arsenic, dead; 1.4279 iodine conversion: coefficient of disulfide. 5.1.5.3 The content of realgar (As,S,) expressed in mass percentage (X,) is calculated according to formula (4): X, = X. X 1.641 9
Wherein: x,
-mass percentage of iodine, %;
coefficient of arsenic conversion to disulfide.
5.1.6 Allowable error
Take the arithmetic mean of the parallel determination results as the final analysis result. The absolute difference of the parallel determination results should not be greater than the allowable error listed in Table 6.
Confirm (As) content
30.0050.00
50. 00~60. 00
5.2 Determination of As content
5.2.1 Method summary
Potassium permanganate method
Table 6 Tolerance
Tolerance
After the sample is decomposed with concentrated sulfuric acid and anhydrous sodium sulfate, it is titrated with potassium permanganate standard titration solution in a strong acid solution with potassium iodate as the catalyst.
5As0,-+2Mn0 +6H+=5As0! -2Mn +3H,05.2.2 Reagents and solutions
5.2.2.1 Anhydrous sodium sulfate.
5.2.2.2 Sulfuric acid (p: 1. 84 g/mL).
5.2.2.3 Hydrochloric acid (p: 1.19 g/ml.). 5.2.2.4 Potassium iodate solution: 0.54 g/L. 5.2.2.5 Potassium permanganate standard solution: (1/5KMnO4) 0.1 mol/L. Prepare and calibrate according to 4.12 of G3/T60J-1988.
5.2.3 Sample
The sample is dried at (80 ± 2)°C for more than 2 hours and placed in a desiccator to cool to room temperature. 5.2.4 Analysis steps
Use the difference method to weigh about 0.25z sample, accurate to 0.0002g, and place it in a 250mL conical flask. Add 2g of anhydrous sodium sulfate GR 17513-1998
(5.2.2.1) and 5mL of sulfuric acid (5.2.2.2), mix thoroughly, and heat at low temperature for about half an hour to decompose the sample. If there is yellow milky sulfur left, gradually increase the temperature until the sulfur at the bottom of the flask disappears, and inject about 3mL of sulfuric acid (5.2.2.2) along the mouth of the flask. Transfer all the sulfur adhering to the bottleneck into the solution, continue heating, and after all the sulfur disappears, carefully add 5mL of distilled water to make it slightly boil with small bubbles continuously. Cool, add 80mL of distilled water, 3mL of hydrochloric acid solution (5.2.2.3), drop potassium iodate solution (5.2.2.4), and use potassium peroxide standard titration solution (5.2.2. 5) The end point is when the pink color does not disappear for 1 minute. A blank test is performed at the same time as the sample determination.
5.2.5 Expression of analysis results
5.2.5.1 The content of A5 (X,) expressed as mass percentage is calculated according to formula (5): X--c(V--Ve) × 0. 037 46 × 100m
Wherein: actual concentration of potassium permanganate standard titration solution.mol/L; V——volume of potassium permanganate standard titration solution consumed by the sample, mL; volume of potassium permanganate standard titration solution consumed by the blank test, ml.; V
m-mass unit of the sample·z:
0. 037 4G-1-to-t.(00 mL potassium permanganate standard titration solution Cc(1/5KMnO,)=1.000 mol/L: equivalent to the mass of arsenic expressed in grams.
5.2.5.2 The content of realgar (As2S,) expressed in mass percentage (X:) is calculated according to formula (3). 5.2.5.3 The content of realgar (AszS) expressed in mass percentage (X;) is calculated according to formula (4). 5.2.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the final analysis result. The absolute difference of the parallel determination results should not be greater than the allowable difference listed in Table 7.
Table 7 Allowable error
Arsenic (As) content
30. 00 ~ 30.30
> 50. 00-~ 60. 0G
5.3 Determination of arsenic trioxide content Melting spot method 5.3.1 Method summary
Allowable error
Use dilute hydrochloric acid to extract arsenic trioxide from the sample. In an acidic solution, use iodine and tin cyanide to reduce the acid to arsenic gel. Add zinc particles to reduce arsenic acid to arsenic hydrogen gas. The arsenic reacts with mercuric bromide test paper to produce a brown-yellow arsenic compound. Compare it with the standard arsenic compound.
5.3.2 Reagents and solutions
5. 3. 2. 1
Hydrochloric acid (p: 1.19 g/ml.).
Hydrochloric acid solution: 5+95.
5. 3. 2. 4
Potassium iodide solution: 200g/L
Hydrochloric acid solution: 100g/L.
Stannoyl chloride solution: 400g/L. Weigh 40g of sodium dioxide, add 50ml of sodium hydroxide (5.3.2.1), heat to dissolve. Dilute to 100ml with water in 5. 3. 2. 5
, shake, add a few metal particles, and stick them in a brown reagent bottle. 5.3.2.6 Seedless zinc particles: 1~-3nm.
5.3.2.7 Evolved mercury test paper: weigh 1.25g of mercury hydrate, dissolve in 25ml of ethanol, put the filter paper strip into this solution for about 1h, then take it out, and store it in a sealed color-coded bottle in the dark for later use. 5.3.2.87 Lead acetate absorbent cotton: Weigh 11.8 lead acetate, dissolve in 100mL water, add a drop of glacial acetic acid, and place absorbent cotton in the solution. After 2 hours, take out and squeeze out the solution. Dry it and prepare GB 17513--1998
5.3.2. 9 standard solution; 100)μg/mL. Weigh 0.1320g of arsenic trioxide (reference reagent) that has been dried at 70~~80℃ for 2 hours in a 100mL beaker, add 2mL of sodium hydroxide solution (200g/L). Stir to dissolve, add a little heavy water and a drop of phenolic acid indicator solution, and add sulfuric acid (0:1.84g/ml.) solution (1:1) until the red color disappears. Then transfer it to a 1000mL volumetric flask, dilute it to the scale with water, and add a pinch. This solution contains 100μg arsenic in 1ml.
5.3.2.10 Arsenic standard solution: 1 μg/mL. Pipette 10 ml of arsenic standard solution (5.3.2.9) into a 100 mL volumetric flask, dilute to the mark with water, and shake well. This solution contains 1 μg of arsenic per ml. 5.3.3 Instruments and devices
5.3.3.1 Iodine analyzer: as shown in Figure 3.
A-saw-shaped bottle, B-mouth cap; C-gas guide arm; D-stopcock: K-stopcock 3 arsenic determination device
A is a 1G0 mL standard ground-mouth conical bottle; B is a hollow standard ground-mouth stopper, connected with a gas guide tube C (outer diameter 8.0 mm, inner diameter 6.0 nm), with a total length of about 1&mm; D is a plexiglass stopper with holes, its upper circular plane has a circular hole in the center, the aperture is consistent with the inner diameter of the gas guide tube C, and its lower aperture is adapted to the outer diameter of the gas guide tube. The pre-end of the gas guide tube C is inserted into the lower hole of the stopcock, and the tube is matched with the circular hole of the stopcock. It is glued and fixed; E is a plexiglass stopcock cover with a circular hole in the center (aperture 6.0 μm), which fits tightly with L). During the test, 60 mg of lead acetate cotton is placed in the tube (the tube height is 60-80 mm), and then a piece of mercuric bromide test paper is placed on the top plane of the stopcock D (the size of the test paper should be such that it can cover the aperture without being exposed outside the plane), and the stopcock cover E is covered and tightened. 5.3.4 Sample
The sample is dried at (80+2)°C for 2 h, placed in a desiccator and cooled to room temperature. 5.3.5 Analysis Step
Weigh 0.9.1 g of the sample to an accuracy of (.00] g and place it in a 250 mL beaker, grind it with a glass pestle, add 20 mL of hydrochloric acid solution (5.3.2.2), 5 ml of hydroxylamine solution (5.3.2.4), and stir continuously for 30) min. Pour the clear solution into a 500 mL volumetric flask and filter it. Treat the severe case 2 times in succession, using 10 mL of hydrochloric acid solution (5.3.2.2) and 2.1 mL of hydroxylamine hydrochloride solution (5.3.2.4) each time, stirring for 10 min, combining the filtrates into a 500 mL volumetric flask, adding water to the mark, and simmering with a spoon. Pipet 10 ml of the filter film into a 10 ml volumetric flask, dilute with water to the mark, shake and pipette 2.0 ml of the liquid into a ground-mouth bottle or conical flask. Add 5 ml of hydrochloric acid (5.3.2.1) and 20 ml of water. Add 5 ml of potassium iodide solution (5.3.2.3), drip stannous chloride solution (5.3.2.5), let it stand for 10 minutes, add 2 g of zinc granules (5.3.2.5), immediately plug the tube containing the filter film into the 10 ml volumetric flask or conical flask, react at 25-40 °C for 1 hour, take out the bromide test paper, and the arsenic stain should not be darker than the standard stain. The standard for comparison with realgar lump is to measure 2.8 ml of the standard solution (6.3.2.10) and treat it in the same way as the sample. The standard for comparison with realgar concentrate is 4.0 mL of the solution (5.3.2.10) and the sample is treated in the same manner. GB 17513-1998
5.4 Determination of Arsenic Dioxide Content Ag-DDTC Method 5.4.1. Summary of Method
Use dilute hydrochloric acid to remove the arsenic dioxide in the sample. In an acid solution, use potassium iodide and stannous nitride to reduce arsenic acid to arsenic acid. Use zinc nitride to reduce the acid to arsine gas, which is absorbed by arsine. Arsenic oxide reduces the arsenic in the reagent to red colloidal elemental silver, which is compared with the standard by visual colorimetry.
5.4.2 Reagents and Solutions
5.4.2.1 Hydrochloric acid (p: 1.19 g/ml.). 5. 4. 2. 2 Hydrochloric acid solution: 5+95
Hydroxylamine hydrochloride solution: 100 g/L
Potassium iodide bath solution: 200 g/L.
Stannous chloride solution: 400 g/L. Weigh 40 g of tin dichloride, add 50 mL of hydrochloric acid (5.4. 2.1), and heat to dissolve. Dilute to 100 uL with 5. 4. 2. 5
water, shake the spoon, add a few grains of metallic tin, and store in a brown reagent bottle. 5. 4.2.6 Arsenic-free zinc particles; 1~3 mm
5. 4. 2. 7
Lead acetate absorbent cotton: Weigh 11.8 B of lead acetate. Dissolve in 100 ml. water, add a few drops of glacial acetic acid, immerse the absorbent cotton in this solution, take it out and squeeze out the free liquid, dry it and set it aside. 5.4.2.8 Arsenic hydrogen absorption: Weigh 0.23 g silver diethyldithiocarbamate (Ag DDTC). Dissolve it with a small amount of dichloromethane, add 3 ml triethanolamine, dilute to 100 mL with dichloromethane, let stand overnight, filter with absorbent cotton. Store the filtrate in a brown bottle. Store in a cool place, effective within two weeks.
5.4.2.9 Arsenic standard solution: 100μ/mL, weigh 0.1320 g of arsenic trioxide (standard reagent) that has been dried at 70-80°C for 2h in a 100 mL beaker, add 2 ml sodium hydroxide solution (200 g/L), stir to dissolve, add a small amount of water and a drop of phenolic acid indicator solution, and add sulfuric acid (p: 1.84 g/ml.) solution (1.+1) to neutralize until the red color disappears. Then transfer to a 1000 ml volumetric flask, dilute to the mark with water, shake well, this solution contains 100 μg of arsenic in 1 mL. 5.4.2.10 Arsenic standard solution: 1 μg/mL, draw 10 mL of arsenic standard solution (5.4.2.9) into a 1000 ml volumetric flask, dilute to the mark with water, shake well, this solution contains 1 μg of arsenic in 1 mL. 5.4.3 Apparatus and device
Arsine gas generation and absorption device, as shown in Figure 4. A is a 100 ml standard mill II conical flask; B is a hollow standard mill port stopper, connected to the air guide tube C (one end has an outer diameter of 8 mm,The inner diameter is 6 mm, the other end is 180 mm long, the outer diameter is 4 mm, the inner diameter is 1.6 mm, and the inner diameter of the tip is 1 mm). D is a flat-bottomed glass tube (180 mm, inner diameter 10 mm, with a scale at 5.0 mL). :
Potential cover 1
uml. Graduation
A-chain bottle; B-mouth stopper: C-
Gas guide tube; D-flat bottom glass tube
Figure 4 Arsenic hydrogen gas generation and absorption device
GB 17513—1998
The absorption tube should be cleaned and dried before use. During the test, 60 mg of lead acetate cotton is placed in the airway C (the height of the tube is about 80 mm), and 5 mL of hydrogen ion absorption liquid is placed in the D tube. 5.4.A Sample Dry the sample at (80 ± 2) °C for more than 2 h, place it in a desiccator and cool it to room temperature. 5.4.5 Analysis Steps Weigh 0.940 g of sample, accurate to 0.001 g, place it in a 250 ml beaker, grind it with a glass pestle, add 20 mL of hydrochloric acid solution (5.4.2.2), 5 mL of hydroxylamine hydrochloride solution (5.4.2.3). Stir continuously for 30 min, pour the solution into a 500 ml volumetric flask and filter it. Treat the precipitation twice in succession. Use 10 mL of hydrochloric acid solution (5.4.2.2), 2 mL of hydroxylamine hydrochloride solution (5.4.2.3) each time, stir for 10 min, combine the filtrate into a 500 mL volumetric flask, add water to the mark, and stir well. Pipet 10.0 mL of the filtrate, transfer it to a 100 mL volumetric flask, dilute it to the mark with water, shake well, and then use a pipette to transfer 2.0 mL of the solution into a conical flask, add 5 mL of hydrochloric acid (5.4.2.1) and 20 mL of water, then add 5 mL of potassium iodide solution (5.4.2.4), and five drops of stannous chloride bath (5.4.2.5). After leaving it at room temperature for 10 min, add 2 g of zinc particles (5.4.2.6), immediately plug the installed gas guide tube C on the male flask, and let the generated hydrogen hydride gas be introduced into tube D to be absorbed by the hydrogen hydride absorption solution. After reacting at 25-40℃ for 45 min, take out tube D, add trinitroform to the mark, mix, and compare with the standard. The color of the resulting solution shall not be darker than that of the standard control solution. If necessary, the measurement can be carried out by spectrophotometer.
The standard for comparison with realgar lump is to measure 2.8 mL of the standard solution of god (5.4.2.10) and treat it in the same way as the sample. The standard for comparison with realgar concentrate is to measure 4.0 mL of the standard solution of monument (5.4.2.10) and treat it in the same way as the sample. 5.5 Determination of moisture
5.5.1 Summary of method
The sample is dried at (8012)°C to constant weight, and the moisture is calculated based on the lost mass. 5.5.2 Instruments
General laboratory instruments and:
5.5.2.1 Weighing bottle; flat, with ground mouth, diameter of about 70 mm, height of about 35 mm. 5.5.2.2 Oven: with automatic temperature controller, 5.5.3 Sample
The sample passes through a 2 tmm standard sieve (GB/T 6003). 5.5.4 Analysis steps
Weigh about 50g of sample, accurate to 0.01g, and place it in a weighing bottle that has been pre-dried at (80±2)℃ to constant weight. Gently shake the weighing bottle so that the sample is evenly spread on the weighing plate, open the bottle cap and place it in an oven at (80±2)℃ to dry for 2h, take out the weighing bottle, cover it with the cap, place it in a desiccator to cool to room temperature, and weigh it. Repeat the operation (drying time is 0.5h) until the difference between the two weighings is no more than 0.02. 5.5.5 Expression of analysis results
The moisture (H,O) (X,) expressed as mass percentage is calculated according to formula (6): X, = (mi -m) X 100
The mass of the sample added to the weighing bottle before drying;
where: m—mass of the sample added to the weighing bottle after drying, and m
m—mass of the sample, g.
5.5.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the final analysis result. The absolute difference of the parallel determination results shall not exceed the allowable difference listed in Table 8.
6 Inspection rules
Points (HO)
3. 0u.8.00
GE17513-1998
Allowable difference
6.1 Take a batch of products with uniform quality, and each batch shall not exceed 20 tAllowance
6.2Each batch of products shall be inspected by the quality inspection department of the production unit. The production unit shall ensure that the realgar and orpiment products supplied meet the requirements of this standard and be accompanied by a quality specification, which includes: product name, product grade, quality index, net weight, delivery date, and the address of the production unit of this standard
6.3The user has the right to conduct quality inspection on the realgar and orpiment products received in accordance with the provisions of this standard. If there is any objection, it shall be raised within 30 days after delivery and the dispute shall be resolved through negotiation.
6.4This standard recommends the use of the "rounded value comparison method" specified in GB/T1250 to determine whether the inspection results meet the requirements of this standard. If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample from twice the amount of packaging boxes (packages) for re-inspection: If it is rational sampling, re-sample according to the provisions of Article 4.1.2.1 and then re-inspect. If only one item of the re-inspection result does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified.
6.5 If the supply and demand parties have disputes over product quality and want to file an arbitration, the arbitration shall be conducted in accordance with the relevant provisions of the Product Quality Law of the People's Republic of China.
7 Marking, packaging, transportation and storage
7.1 Lump-shaped high-quality products are packed in wooden boxes lined with leather paper, with a net weight of (50-0.5) kg or (25 ± 0.25) kg. Lump-shaped first-class products and upgraded products are packed in double-layer hemp, with a net weight of (50-0.5) kg; flotation concentrate products are packed in plastic woven bags (GB/T8947), with a net weight of (25 ± 0.25) kg, and the average net weight is not less than 25 kg or 50 kg. 7.2 The package shall indicate the product name, product grade, net weight, this standard number, production unit and address. 7.3 During transportation, realgar and orpiment products should be protected from moisture, heat and packaging damage. 7.4 Realgar and orpiment products should be stored in well-ventilated warehouses. 8 Safety
Realgar and orpiment products are sulfide minerals and should not be mixed with strong oxidants.Immediately plug the installed gas guide tube C on the male bottle, so that the generated hydrogen ions gas is introduced into the tube D and absorbed by the hydrogen ions absorption liquid. After reacting at 25-40℃ for 45 ml, take out the tube D, add triazine to the scale, mix, and compare with the standard. The color of the resulting solution shall not be darker than that of the standard reference solution. If necessary, it can be measured with a spectrophotometer.
The standard for comparison with realgar lump is to measure 2.8 mL of the standard solution (5.4.2.10) and treat it in the same way as the sample. The standard for comparison with realgar concentrate is to measure 4.0 mL of the standard solution (5.4.2.10) and treat it in the same way as the sample. 5.5 Determination of moisture
5.5.1 Summary of method
The sample is dried at (8012)℃ to constant weight, and the moisture is calculated based on the lost mass. 5.5.2 Instruments
General laboratory instruments and:
5.5.2.1 Weighing bottle; flat, with ground mouth, diameter about 70 mm, height about 35 mm. 5.5.2.2 Drying oven: with automatic temperature controller, 5.5.3 Sample
The sample passes through a 2 tmm standard sieve (GB/T 6003). 5.5.4 Analysis steps
Weigh about 50g of sample, accurate to 0.01g, and place it in a weighing bottle that has been pre-dried at (80±2)℃ to constant weight. Gently shake the weighing bottle so that the sample is evenly spread on the weighing pan, open the bottle cap and place it in an oven at (80±2)℃ to dry for 2h, take out the weighing bottle, cover the bottle cap, place it in a desiccator to cool to room temperature, and weigh it. Repeat the operation (drying time is 0.5h) until the difference between the two weighings is no more than 0.02. 5.5.5 Expression of analysis results
The moisture (H,O) (X,) expressed as mass percentage is calculated according to formula (6): X, = (mi -m) X 100
The mass of the sample added to the weighing bottle before drying;
where: m—mass of the sample added to the weighing bottle after drying, and m
m—mass of the sample, g.
5.5.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the final analysis result. The absolute difference of the parallel determination results shall not exceed the allowable difference listed in Table 8.
6 Inspection rules
Points (HO)
3. 0u.8.00
GE17513-1998
Allowable difference
6.1 Take a batch of products with uniform quality, and each batch shall not exceed 20 tAllowance
6.2Each batch of products shall be inspected by the quality inspection department of the production unit. The production unit shall ensure that the realgar and orpiment products supplied meet the requirements of this standard and be accompanied by a quality specification, which includes: product name, product grade, quality index, net weight, delivery date, and the address of the production unit of this standard
6.3The user has the right to conduct quality inspection on the realgar and orpiment products received in accordance with the provisions of this standard. If there is any objection, it shall be raised within 30 days after delivery and the dispute shall be resolved through negotiation.
6.4This standard recommends the use of the "rounded value comparison method" specified in GB/T1250 to determine whether the inspection results meet the requirements of this standard. If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample from twice the amount of packaging boxes (packages) for re-inspection: If it is rational sampling, re-sample according to the provisions of Article 4.1.2.1 and then re-inspect. If only one item of the re-inspection result does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified.
6.5 If the supply and demand parties have disputes over product quality and want to file an arbitration, the arbitration shall be conducted in accordance with the relevant provisions of the Product Quality Law of the People's Republic of China.
7 Marking, packaging, transportation and storage
7.1 Lump-shaped high-quality products are packed in wooden boxes lined with leather paper, with a net weight of (50-0.5) kg or (25 ± 0.25) kg. Lump-shaped first-class products and upgraded products are packed in double-layer hemp, with a net weight of (50-0.5) kg; flotation concentrate products are packed in plastic woven bags (GB/T8947), with a net weight of (25 ± 0.25) kg, and the average net weight is not less than 25 kg or 50 kg. 7.2 The package shall indicate the product name, product grade, net weight, this standard number, production unit and address. 7.3 During transportation, realgar and orpiment products should be protected from moisture, heat and packaging damage. 7.4 Realgar and orpiment products should be stored in well-ventilated warehouses. 8 Safety
Realgar and orpiment products are sulfide minerals and should not be mixed with strong oxidants.Immediately plug the installed gas guide tube C on the male bottle, so that the generated hydrogen ions gas is introduced into the tube D and absorbed by the hydrogen ions absorption liquid. After reacting at 25-40℃ for 45 ml, take out the tube D, add triazine to the scale, mix, and compare with the standard. The color of the resulting solution shall not be darker than that of the standard reference solution. If necessary, it can be measured with a spectrophotometer.
The standard for comparison with realgar lump is to measure 2.8 mL of the standard solution (5.4.2.10) and treat it in the same way as the sample. The standard for comparison with realgar concentrate is to measure 4.0 mL of the standard solution (5.4.2.10) and treat it in the same way as the sample. 5.5 Determination of moisture
5.5.1 Summary of method
The sample is dried at (8012)℃ to constant weight, and the moisture is calculated based on the lost mass. 5.5.2 Instruments
General laboratory instruments and:
5.5.2.1 Weighing bottle; flat, with ground mouth, diameter about 70 mm, height about 35 mm. 5.5.2.2 Drying oven: with automatic temperature controller, 5.5.3 Sample
The sample passes through a 2 tmm standard sieve (GB/T 6003). 5.5.4 Analysis steps
Weigh about 50g of sample, accurate to 0.01g, and place it in a weighing bottle that has been pre-dried at (80±2)℃ to constant weight. Gently shake the weighing bottle so that the sample is evenly spread on the weighing pan, open the bottle cap and place it in an oven at (80±2)℃ to dry for 2h, take out the weighing bottle, cover the bottle cap, place it in a desiccator to cool to room temperature, and weigh it. Repeat the operation (drying time is 0.5h) until the difference between the two weighings is no more than 0.02. 5.5.5 Expression of analysis results
The moisture (H,O) (X,) expressed as mass percentage is calculated according to formula (6): X, = (mi -m) X 100
The mass of the sample added to the weighing bottle before drying;
where: m—mass of the sample added to the weighing bottle after drying, and m
m—mass of the sample, g.
5.5.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the final analysis result. The absolute difference of the parallel determination results shall not exceed the allowable difference listed in Table 8.
6 Inspection rules
Points (HO)
3. 0u.8.00
GE17513-1998
Allowable difference
6.1 Take a batch of products with uniform quality, and each batch shall not exceed 20 tAllowance
6.2Each batch of products shall be inspected by the quality inspection department of the production unit. The production unit shall ensure that the realgar and orpiment products supplied meet the requirements of this standard and be accompanied by a quality specification, which includes: product name, product grade, quality index, net weight, delivery date, and the address of the production unit of this standard
6.3The user has the right to conduct quality inspection on the realgar and orpiment products received in accordance with the provisions of this standard. If there is any objection, it shall be raised within 30 days after delivery and the dispute shall be resolved through negotiation.
6.4This standard recommends the use of the "rounded value comparison method" specified in GB/T1250 to determine whether the inspection results meet the requirements of this standard. If one of the indicators in the inspection results does not meet the requirements of this standard, re-sample from twice the amount of packaging boxes (packages) for re-inspection: If it is rational sampling, re-sample according to the provisions of Article 4.1.2.1 and then re-inspect. If only one item of the re-inspection result does not meet the requirements of this standard, the entire batch of products shall be judged as unqualified.
6.5 If the supply and demand parties have disputes over product quality and want to file an arbitration, the arbitration shall be conducted in accordance with the relevant provisions of the Product Quality Law of the People's Republic of China.
7 Marking, packaging, transportation and storage Www.bzxZ.net
7.1 Lump-shaped high-quality products are packed in wooden boxes lined with leather paper, with a net weight of (50-0.5) kg or (25 ± 0.25) kg. Lump-shaped first-class products and upgraded products are packed in double-layer hemp, with a net weight of (50-0.5) kg; flotation concentrate products are packed in plastic woven bags (GB/T8947), with a net weight of (25 ± 0.25) kg, and the average net weight is not less than 25 kg or 50 kg. 7.2 The package shall indicate the product name, product grade, net weight, this standard number, production unit and address. 7.3 During transportation, realgar and orpiment products should be protected from moisture, heat and packaging damage. 7.4 Realgar and orpiment products should be stored in well-ventilated warehouses. 8 Safety
Realgar and orpiment products are sulfide minerals and should not be mixed with strong oxidants.4. Orpiment and orpiment products should be stored in a well-ventilated warehouse. 8. Safety
Orpiment and orpiment products are sulfide minerals and should be avoided from mixing with strong oxidants.4. Orpiment and orpiment products should be stored in a well-ventilated warehouse. 8. Safety
Orpiment and orpiment products are sulfide minerals and should be avoided from mixing with strong oxidants.
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