GB/T 8151.1-2000 Chemical analysis methods for zinc concentrates - Determination of zinc content
Some standard content:
ICS73.060
National Standard of the People's Republic of China
GB/T8151.1—2000
Methods for chemical analysis of zinc concentrate
Determining zinc content
Methods for chemical analysis of zine conccntratesDetermining zinc content
Published on 2000-02-16
Implemented on 2000-08-01
State Administration of Quality Supervision, Inspection and Quarantine
1/T8:51.1—2000
This standard adopts a new chemical analysis method to determine the content of zinc in concentrate. 1.1.1987 Chemical analysis method for ore determination - NELTA titration method - is a revision of the main contents of the NELTA standard titration method, which is a tailored method: Method 2 ... B/T14571978 Chemical Analysis of Metallurgical Products - General Principles and Items of Standard 61/T173-1006 and Basic Terminology of Chemical Analysis of Products are not standardized and shall be in effect from the date of implementation. B/5.1-187. This standard is proposed by the State Administration of Metallurgy: This standard is drafted by the China National Nonferrous Metals Industry Standard Metrology and Quality Research Institute and the China Nonferrous Metals Industry Standards Institute. This standard is drafted by Hudang Road Slaughterhouse:
This standard method 1 Main personnel
Dian Guangyu, Xue Gan Pian, the method is drafted by Zhao Xiujuan, Li Shi. Lao Zhou
1 Fan Chen
National Standard of the People's Republic of China
Chemical Analysis Method of Zinc Concentrate
Determination of Zinc Content
Method fer chenieil analvsis l zinr cwacenlnites-Lelermiatiun of zine eonteatGE/T8151.1-7000
Generation #03T8151,1-17
Method 1 Determination of zinc content by EDTA titration with precipitation The standard specifies the determination method of zinc content in ore. The standard applies to the following determination of zinc content in ore. Determination range: 30.00~60.00%. 2 Method summary
The test is carried out with hydrochloric acid, sulphuric acid and sulfuric acid Acid partly decomposed, high-purity, manganese, etc., the presence of elements, the agent in the liquid according to the onion to collect a small amount of dry elements. In the pH 15--E sodium aldehyde-acid solution, with dioxin as the indicator, 1 NxELTA standard solution was determined. The male was removed by the amount of the mixture, but it was early. 3 test
3.1 oxidation
3.2 anti-ascorbic acid,
3.3 ethyl anhydrous).
hydrochloric acid 1.1.
1.m
perhydrogen acid (e1.67x/m)
ammonia water. 90g/mL).
Z brew (1.0 g/m!.)
Hydrochloric acid: 1+
Sulfuric acid (111)
Sulfuric acid (+s).
Water (1-1):
Washing paint wave: Chemical chain 1) Water 4 boxes of hydrogen water (.7 mixed. Sulfur residue (253/L), prepared at the mouth. Potassium oxide solution (2C0g/).), busy in plastic bottle 3.16
Sodium end acid rate filter ().
Acetic acid-sodium sulfate solution 115:1 EG acetic acid (3.3) dry water, add 18: acetic acid (3.8) dilute with water 3.17
to 1000ml mixed spoon.
National Quality and Technical Supervision Bureau 2000-02-16 approved 2000-08-01 welcome
GB/1 8151. 1---2099
3.18 Iron solution (:002/1.) Weigh [cGg solution: 1000mI. Density 13.111.3.19 Base (0.5g/1.
3.20 All three reagents are used within the limit of 3.212 Amine 2-acid cobalt EDTA smelt solution (CHN.N: 3H,U) = W/]. 3.21. Preparation: Weigh 18. 6 ethylenediamine pyrrolidone diacetate. Heat the mixture in water, cool until wet, transfer 10 ml, dilute with water, place in the bottom mud, and then calibrate 3.21.2 Calibration: weigh 0.100 g of polymetallic acid (9.99%) in a 400 μl beaker. Add 10 g of hydrochloric acid (3.3 μl), dissolve according to the pressure, remove and cool, add 25 ml, mL iron content 5.12 ml, and perform the following according to 8.2 to 5.3.5. Perform the test in the air, calculate the stability coefficient of the standard titration solution for light according to the formula: P\wV:
Formula: FNa: The stability coefficient of the EDTA standard titration solution: - The amount of residual liquid:
The volume of the standard EDTA solution consumed during the calibration, mL; V - The volume of the new EDTA standard titration solution consumed during the calibration, NE: The volume of the EDTA standard titration solution, mI. ?1| |tt||Take the average titration coefficient of three calibrations, and the range of the three calibrations should not exceed 0.000008/mT. Otherwise, the new standard is,
4 Test sample
4.1 The sample should pass through a 1.100m mesh sieve,
1. The sample should be placed at 55-5 for 1h, cooled to room temperature in a desiccator, and the step is
5.1 Test sample
slowly take 0.2 3. 3001 Test material:
Perform a single test and take the half-mean value. 5.2 Blank test method
Perform a blank test with the test material.
5.3 Determination
5.3.1 Place the test material 1 in a 46 ml cup, add a little water to moisten the solution, add 0.3 ml of sodium ions, add 10 ml of sodium ions, and grind all the materials. After the test material is fully dissolved, add sodium ions, and add 5 ml of sodium ions. (3) Continue to heat the sample until the sample has a high content of iron. Remove the sample when it is steamed until it has a low content of iron. Remove the sample and cool it down. Add 2-3% high oxygen and continue heating until the sample is heated to a low content of iron. Remove the sample and cool it down. Add 2-3% high oxygen and continue heating until the sample is heated to a low content of iron. Add 2-3% high oxygen and add 2-3% high oxygen. Add 2-3% high oxygen and add 2-3% high oxygen. Cover the sample with sodium ions, remove the sodium ions, remove the sodium ions, and remove the sodium ions. Add 2-3% high oxygen and add 2-3% high oxygen ... The furnace is convenient for storage in Hong Kong and is about 20 stations), 5.3.2 3-5 oxidation money, 5m). Pass the waist and press it down. Use the magic (.?) to completely wash the initial starch, then add 10m). If the heat is slightly boiling for 1-2.n, the whole hot knife quickly qualitatively heats the paper and washes the new precipitate in the beaker with hot paint for 2~.3 seconds, and there is no guarantee that 5.3.3 will use hot selected waves to wash the precipitate in the beaker of the original sediment, and the class salt load (3.9) will help the effect, add 1ml. Ammonium hydroxide liquid, neutralize with ammonia.7 until the precipitate is completely shrunk, excess 101, heat slightly 1~2mim, remove the selected original paper, retain the liquid in the beaker, and use hot waves to wash the beaker and the anti-sedimentation for 1 time. 5.3.4 will be on the business (5, 3 flow belt and liquid shrink lathe! 133ml of the drug is thoroughly cooled in a mixing bowl; add 5.3.5ml of 0.1ml of ascorbic acid-isocyanate, 5.1ml of water, 13.3ml of hydrochloric acid until the solution turns red; add 2ml of acetic acid-sodium chloride solution, 51ml of potassium fluoride, 10ml of sodium thiocyanate solution, add 2 drops of GB/T 5151. 1--2000
indicator, and add N:FETA indicator until the solution turns from purple-red to dark brown, which is the end point. 6 Expression of analysis results
Calculate the percentage of zinc by the formula:
FV-x103 cd%0.5816
Formula: F...-N.H14 standard titration box for zinc standard determination system /ml.W-reduced liquid NaEDTA standard agreed liquid volume, ml.V test monitoring solution N, EDTA standard agreed floating limit volume nT: -·Test material quality requirements,
steel quantity is converted into a quantitative system effect
-51.& The measured fraction
is expressed as a two-digit small effect.
? The difference between the actual amount of the product and the actual amount of the product is 1
5o, 3f.-4n, n0
4n, ~An
25f, f~.nn nm
Extraction and separation NaEDTA titration method for determination of zinc
Method 2
8 Standard specification
rate standard specifies the detailed determination method. This standard applies to the general regulations for medium-containing concentrates: the specified range is 11.(0-62.00. Summary of the method
The sample pieces are cooled and then cut again. Some of the samples are not checked for high chlorine content. The sulfur and lemon salts are not used. The detailed information of the compound is obtained by printing and opening the car. When the content is large, the product is separated and the zinc content is determined by titration method A at H5.5. 1C reagent
19. 1 drop of abdominal -
13.2 Zhongming.
15.3 Anhydrous ethanol.
13.4 Aldehyde. 1.14m)
Nitric acid (1.42 g/mL)
Hydrogen peroxide (1.13 g/aL)
Southern acid 01.54 g/mL
Ammonia water (908/1)
10.9Hydrochloric acid + 4).
10.1nSodium chloride solution (23p1.
10.11Yamashita solution 1GC/
10.12Qibeizhou solution ([500 g/1.)
GB/T8151, 1-2000
10.13 drag the whole system 50 with pig, 1cu = nucleic acid hydrogen, 200 paper teaching relatively swim in the solution in the well to choose 1c00l-m. must pass the soul
10.14 jump road reduction: special 253 multi-ring six times the national rubber (black road lamp product down in the door 60 certificate 7 alcohol (01.04R/cL ）Then take ￥10001..10.15 fast storage solution (45/L): 4 = sign nitric acid chopsticks \ FVC,)-0H solution in water and release to 1uU0ml. 1016 front electrode (01) put dimethyl S92 potassium nitrate parts and use in the blood to grind when the amount of the package is consistent with the filter:
1017Z two glue four Z accompany two books (NaTA standard elimination according to cCHiNO.Na HO)-.5o!/10.17.1! System, you take 18.65 ethylenediaminetetraacetic acid dihydrate, slightly heat decompose in water, cool until firmly wet, transfer to a 110m volume bottle: use Yongda to release to the scale. After three days of stabilization 10.17.2 calibration: take a portion of gold zinc SS.99% (the size of the mass plate is close to the life of zinc in the test grid, the error is 00001, put it in a different In the shape of the image, add 15 mL of 1:1 m 2 HCl and 8.35 mL of EDTA (3.15 mL of EDTA). After decomposition, boil and release oxygen dioxide. Cool and dilute with water in a 500 mL chamber. The following steps are carried out according to 12.3.2 to 2.3.3. The volume of the NHTTA standard solution is determined by the method as V. 1 V is used to calculate the Na:EDTA standard solution coefficient. Formula 3 is applicable to each ring. F. = ni./V.in= [ -- :
In the formula, F is the titration coefficient E of the NaEDTA standard solution; V is the volume of the VanYrA standard titration solution consumed during calibration, Ir.L. River - I belong to the plate of Shu g.
Half a line of ring determination. Fang,,.: The total change of C.CC3C1s/mL needs to be changed: No, the average titration coefficient is calculated by formula (1),
F=(F. +FF/
11 Test sample
11.1 The sample should pass through a .Jmm mesh sieve.
11.2 The sample should be pre-cooled to room temperature at 108°C in a desiccator. 12.1 Test sample
Weigh 2.1., G1. The sample
is tested twice independently and the average value is collected. 12.2 Width concave testWww.bzxZ.net
With the sample efficacy test:
12.3 Determination
12.3.1 Put the sample (12.1) into a 300ml bottle, add 20% water, 2-3 ℃, react at room temperature for 5 ℃ without stirring. Put it in a 15 ℃ oven and heat it in an electric furnace. The natural gas must be driven away. After cooling, add 155 L water, return to heat and boil, control: if the sample is completely dissolved, transfer the test solution to 5W0 r:T. volumetric bottle + clean the bottom of the push bottle. Use water to filter until effective! Otherwise, use this paper to pass the solution to m, the volumetric flask with water to pass the material on the paper, put the filtered material in 25 platinum cut, and then put it into 5 and expand it for I, then 2 hydrogen chlorine, 5GB/T 815'.1—20CC
high chlorine, blow until aerobic acid smoke is released, cool, cut, dilute, right mountain lead sulfate precipitation needs to be returned: transfer the energy solution to the entire plate on the test volume, wash the lack, filter into the volume, and then weigh the water group until the quarter. 12.3.2 Transfer 000 (12..1250. The most turbid product is collected from the liquid droplet, add 3m. dilute salt carrier (16.! 5UmL energy: fully mixed. Then add 3al isopentyl ketone. Then report the drug 1mi. After the material is separated, the lower layer is effectively added to another concentrated disease bucket, such as 2) methyl cation, half of the first extraction, after the phase separation, discard the first aqueous phase, and add two organic phases. The total number of people is 0Fml. The case is bad, and the two fractions are added to 1mL dilute plate (10.9) 79m ethyl rain balance bottom medicine. After the liquid in the must be added to the "Da Huan machine 12.3. According to the child, add 1cm!. Sodium hydroxide solution, lun:L dangerous solution, 2u =nL short liquid, 3m1. iodine solution, t. [ g-1 test, open NETA standard fixing solution, when the color of the needle turns from red to yellow, record the effective time V: 3 Expression of analysis results
According to the formula:
Zm(% = r(V-) 1
Na, EDTA standard fixing solution to the determination coefficient: tl. In particular:
1.--N during the titration test; 2. The volume of EDTA standard fixing solution: TmT.W.---The volume of NETA standard fixing solution consumed by the titration sample m[..Y12g]. The new result should be shown in the decimal place
14 The allowable difference
The value of the inter-laboratory analysis standard should be greater than the specified working permit r=2. 8M (S -5 /2:
Formula: 5016: i0339.Previous laboratory standard deviation S.=,01G.032 (S.scarce - laboratory coefficient;..= (+)2 (i.e. the final result is average).99% (mass disk size virtual and test grid zinc life Gua, error 00001, placed in a different dimension,! Lower mass. 1m 15mL succinic acid 8.35mL fast death storage (3.15 decomposition after boiling, release of oxygen dioxide, cool eyebrows with water dilution room 500m1. The following according to 12.3.2 ~: 2.3.3 system, the method of determining the body of NHTTA standard fluid is V, 1V calculation Na: EDTA standard determination coefficient of Liu shovel. For each ring applicable to the formula: 3), F. = ni./V.in = [ -- :
In the formula, F is the titration coefficient E of the NaEDTA standard solution; V is the volume of the VanYrA standard titration solution consumed during calibration, Ir.L. The total change in C.CC3C1s/mL needs to be changed: No, the average titration coefficient is calculated by formula (1),
F=(F. +FF/
11 Test sample
11.1 The sample should pass through a .Jmm mesh sieve.
11.2 The sample should be pre-cooled to room temperature at 108°C in a desiccator. 12.1 Test sample
Weigh 2.1., G1. The sample
is tested twice independently and the average value is collected. 12.2 Width concave test
With the sample efficacy test:
12.3 Determination
12.3.1 Put the sample (12.1) into a 300ml bottle, add 20% water, 2-3 ℃, react at room temperature for 5 ℃ without stirring. Put it in a 15 ℃ oven and heat it in an electric furnace. The natural gas must be driven away. After cooling, add 155 L water, return to heat and boil, control: if the sample is completely dissolved, transfer the test solution to 5000T. Clean the bottom of the volumetric bottle. Dilute with water until effective! Otherwise, use medium paper to filter the solution to 10000T, use water to filter the substance on the volumetric bottle, place the filtered substance in 25000T, and then put it into 5000T for decomposition, then add 20000T of hydrogen chlorine, 50000T. 815'.1—20CC
High chlorine, wind to release oxygen acid smoke, cold printing, scratch,, technique dilute cup, right mountain lead sulfate precipitation filter needs to be returned: transfer the energy liquid to the upper volume, wash the lack of special, filter into the volume, and then weigh the water group to the minute. 12.3.2 Transfer 000 (12..1250. The liquid drips from the car with the most turbid product, add 3m. dilute salt (16.! 5UmL energy agent: fully mix. Then add 3al base isopentyl Ketone. Then report the drug 1mi. Wait for the material to be separated, the lower layer of the effective person is another concentrated disease bucket, such as 2) methyl form anion, half of the extraction, wait for the material phase separation, discard the first aqueous phase, and two organic. Total person 0Fml. Case bad, add 1mL dilute plate (10.9) 79m ethyl rain balance bottom drug after the necessary south bucket in the liquid into the "Da Huan machine 12.3. According to the child add 1cm!. Sodium dissolution, lun: L dangerous taste dissolution, 2u =nL short-circuit solution, 3 ml iodine solution, t. [g-formaldehyde test, open NETA standard fixing solution, when the color of the titration needle turns from red to yellow, write down the effective value V:3 Expression of analysis results
According to the formula:
Zm(% = r(V-) 1
Na, EDTA standard fixing solution relative to the determination coefficient,: tl. Including:
1.--the ratio of consumption during titration test N2. The volume of EDTA standard fixing solution: TmT.W.---the volume of NETA standard fixing solution consumed by the titration sample m[..Yl2g
the mass of the sample.
The new result is shown in the figure. The allowable difference between the two laboratories should be greater than the specified working standard. The value should be r=2.8M (S -5 /2:
formula: 5016: i0339. The standard deviation of the previous laboratory is S.=,01G.032 (S. - laboratory standard;..= (+) 2 (i.e. the final result is average).99% (mass disk size virtual and test grid zinc life Gua, error 00001, placed in a different dimension,! Lower mass. 1m 15mL succinic acid 8.35mL fast death storage (3.15 decomposition after boiling, release of oxygen dioxide, cool eyebrows with water dilution room 500m1. The following according to 12.3.2 ~: 2.3.3 system, the method of determining the body of NHTTA standard fluid is V, 1V calculation Na: EDTA standard determination coefficient of Liu shovel. For each ring applicable to the formula: 3), F. = ni./V.in = [ -- :
In the formula, F is the titration coefficient E of the NaEDTA standard solution; V is the volume of the VanYrA standard titration solution consumed during calibration, Ir.L. The total change in C.CC3C1s/mL needs to be changed: No, the average titration coefficient is calculated by formula (1),
F=(F. +FF/
11 Test sample
11.1 The sample should pass through a .Jmm mesh sieve.
11.2 The sample should be pre-cooled to room temperature at 108°C in a desiccator. 12.1 Test sample
Weigh 2.1., G1. The sample
is tested twice independently and the average value is collected. 12.2 Width concave test
With the sample efficacy test:
12.3 Determination
12.3.1 Put the sample (12.1) into a 300ml bottle, add 20% water, 2-3 ℃, react at room temperature for 5 ℃ without stirring. Put it in a 15 ℃ oven and heat it in an electric furnace. The natural gas must be driven away. After cooling, add 155 L water, return to heat and boil, control: if the sample is completely dissolved, transfer the test solution to 5000T. Clean the bottom of the volumetric bottle. Dilute with water until effective! Otherwise, use medium paper to filter the solution to 10000T, use water to filter the substance on the volumetric bottle, place the filtered substance in 25000T, and then put it into 5000T for decomposition, then add 20000T of hydrogen chlorine, 50000T. 815'.1—20CC
High chlorine, wind to release oxygen acid smoke, cold printing, scratch,, technique dilute cup, right mountain lead sulfate precipitation filter needs to be returned: transfer the energy liquid to the upper volume, wash the lack of special, filter into the volume, and then weigh the water group to the minute. 12.3.2 Transfer 000 (12..1250. The liquid drips from the car with the most turbid product, add 3m. dilute salt (16.! 5UmL energy agent: fully mix. Then add 3al base isopentyl Ketone. Then report the drug 1mi. Wait for the material to be separated, the lower layer of the effective person is another concentrated disease bucket, such as 2) methyl form anion, half of the extraction, wait for the material phase separation, discard the first aqueous phase, and two organic. Total person 0Fml. Case bad, add 1mL dilute plate (10.9) 79m ethyl rain balance bottom drug after the necessary south bucket in the liquid into the "Da Huan machine 12.3. According to the child add 1cm!. Sodium dissolution, lun: L dangerous taste dissolution, 2u =nL short-circuit solution, 3 ml iodine solution, t. [g-formaldehyde test, open NETA standard fixing solution, when the color of the titration needle turns from red to yellow, write down the effective value V:3 Expression of analysis results
According to the formula:
Zm(% = r(V-) 1
Na, EDTA standard fixing solution relative to the determination coefficient,: tl. Including:
1.--the ratio of consumption during titration test N2. The volume of EDTA standard fixing solution: TmT.W.---the volume of NETA standard fixing solution consumed by the titration sample m[..Yl2g
the mass of the sample.
The new result is shown in the figure. The allowable difference between the two laboratories should be greater than the specified working standard. The value should be r=2.8M (S -5 /2:
formula: 5016: i0339. The standard deviation of the previous laboratory is S.=,01G.032 (S. - laboratory standard;..= (+) 2 (i.e. the final result is average).
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