GB/T 8639.2-1988 Chemical analysis methods for vanadium - The diphenylcarbohydrazide photometric method for the determination of chromium content

This standard is applicable to the determination of chromium content in metallic vanadium. Determination range: 0.004% to 0.20%. This standard complies with GB 1467-78 "General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products". GB/T 8639.2-1988 Chemical Analysis Method for Vanadium - Determination of Chromium Content by Diphenylcarbohydrazide Photometric Method GB/T8639.2-1988 Standard Download Decompression Password: www.bzxz.net

National Standard of the People's Republic of China
Vanadium Chemical Analysis Method
Diphenylcarbonyl Dithiocyanate Spectrophotometric Method for Determination of Chromium Content VandFum - Thetanladinn af
shroanium wuntanl UiubwovkarbazkdaLpctbr pgholkomelckc method
Standard for determination of metal content in China, recommended for determination: 0.0+20 coupons, DDC 669.282
-543062
GE 8639.2--82
General principles and specifications for the safe chemical analysis of properties of products》1. Summary of the method
The test method is to use a mixture of tri-methoxy-1-ol and tri-methoxy-1-ol reagents to separate the components, at 0.160°C for 30 min, and measure the absorbance at a spectrophotometer. The water used for the preparation and analysis is secondary sieves. 2.1 Trichlorodecane,
2.2 Peroxide,
2.3 Anhydrous phosphite.
2.4 Hydroxyethyl ether (1:1 2),
optimal number HSO,—1InolL: high%,
2. Acid (1 high play.
2.7 Acid 1.42gmL2, system.
2. Self-calculated period of chemical creation filter (20 poly) - system ethylene re-ten, 2.9 organic chemical solution of low cost euoH) = t.1nul/
2.10 Thickness reduction 10%
High induction potassium hydroxide solution (0.1%).
Acid fast according to the need ([),
2.13 Steel formula judgment environment heart%! , when collected, over repair out tears. 1,2-dibenzoylmethane ester (0.25%), weigh n. 25 g dibenzyl carbonyl ester (4D ms), example TH, micro, 2.14
2-15 estimate standard Sa:
2.15. Take 2829 first: 10% under 2 volume record can get the standard test, with too much degradation, into 100ml water bottle with water to. Promote, fall: 1 s2-15.2 take 1hml standard degradation solution (% 15.1) ten 00mL complexing agent, uL (2.51, add 0.2g yuan first grid original one price into 1 grid, water,: m|| tt||China will be the color gold industry general company 1988-0111 approval 1989-01-01 buy #
spectrophotometer,
4 sample
test should be through the 3.151mm sieve.
5 analysis step
5. test group
you 0.2550 test
5.2 white test
accompanying the sample to adjust the blank test,
CB 8658.288
5.3.1 Place sample 1) in a 2-mL beaker, add 10 mL of 2.6, and obtain the reaction image. Add 25 mL of (2.4), add 1 to 2 mL of acid, remove and cool, add 5 mL of water to the whole beaker: heat to dissolve the acid. Add about C.6 mL of acid (?.3 Oxidize vanadium, heat to boil, remove and cool to room temperature, add to a volumetric flask, dilute with water to the system, and record the spoon.
5.3.2 Add 20.30 mL of test solution (b.3.1) in a 12 mL diverter, add 1 mL of water, [1. Copper iron test (2.13) 15 mL of trihydrogen monohydrate (2.1), shake immediately for 1 to 2 minutes, let stand and separate, remove the organic phase, and then add 5 mL of copper iron or reagent (2. 13) Add 10 mL of chloroform (2.1).1. ... mL nitric acid (2.7). Heat the mixture at room temperature, remove and cool slightly, add 201. water, heat to dissolve the salts, remove and cool to room temperature, 5.5.4 adjust the pH to 2~-2 with sodium oxide. Add 5mL sulfuric acid (2.5) dropwise as high-chain potassium sulfate (2.11) until the solution appears red, keep for about 2 minutes, 5.-7 minutes, then the solution is complete, cool to room temperature, add 5mL sodium hydroxide solution (2.12), and continue to stir for 5 minutes. Add dropwise sodium hydroxide solution (2.12) until the red color disappears. 5.3.5 transfer to a 5.3.4 mL variable volume bottle, adjust the volume to about 10mL, 1.3mL carbon dioxide (2.[4) and dilute the sample to the mark with water, the effect is very good. 5.3. Put part of the discarded liquid (6.3.5) into 1.5 or 3 mL of blood. Take the empty space obtained by the test as an example, and use a photometer to measure the warm light at a wavelength of nm. Find the corresponding product from the surface line: 5.4 Working procedure
5.1.1 Take 0.500 g of pure gold (minus the gold without gold) and place it in a 200 mL flask. Add 20 mL of mineral acid (2.6), cover with blood immediately, wait for the reaction to stabilize, and add 3 mL of Ethyl acetate (2.4) + 1.2 mL of sodium sulfoxide (2.6). Press b. 3.1 Operation, transfer 20nl, volume 1, with water sieve scale · slide
5-4.2 part of the amount of 0.004% ~ 0.020%. Draw the standard line: transfer 20.00mL test solution (5.1.1) six parts, respectively placed in - 126n.L full bucket, respectively into 0.0.2.4c..60, 0.8D..0m standard solution (2.15.2), with water to 35 into 1. Ask the test line! 2.13: The following 5.2 ~ 3.5 operations, part of the drop can be put into 3m blood bag, with equal degree as north, the light convergence plan involved in the 310m of the length of the measurement of its absorption ratio, with the amount of correction as the loss coordinate, the absorption degree as the ordinate will be the working H. 5.4.5 Preparation of the colorimetric curve containing 0.2~-0.24% of the product. Take 26.00mL solution (5.17 portions) and divide into 12:mL separatory funnels. Add 0, 1.00, 2.0D, 4.30, 600, 8.00 and 16.0Gr.L of chromium standard (2.15.2) respectively. Dilute to 86mL with 322mL of GE 8639-288 water. Add 1mL of standard reagent (3.13). Follow the steps in 5.3.2~5.3.5. Move the colorimetric curve to 0.5cm. Take the quartz crystal as reference. Measure the absorbance of the sample at the place where the colorimetric curve is added with a spectrophotometer. Take the solution as the reference and the absorbance as the ordinate.
B Calculation of analysis results
Calculate the analysis results according to formula (1):
In the formula, m-bzxZ.net
is the sample volume, s:
,--test solution ratio.
Analysis results are expressed as follows.
7 Allowable differences in analysis results between laboratories should not be greater than the allowable differences shown in the following table. 0.304 0, 0, 011 2-0.110~ U, 05 tt t.50-~U, 12C>0.120~0,200 Additional remarks: This standard was drafted by Jinzhou Iron and Steel Co., Ltd. This standard was drafted by Jinzhou Iron and Steel Co., Ltd. The main contributors are Mr. Xie Xianshen and Mr. Wang Fengxiang. 0 tt t.02
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