JB/T 7519-1994 Analysis methods for hazardous solid wastes from heat-treated salt baths (barium salts, nitrate salts)
Some standard content:
Machinery Industry Standard of the People's Republic of China
JB/T 7519-94
Analysis method for hazardous solid wastes from heat treatment salt baths (barium salts, nitrate salts)
Published on October 25, 1994
Ministry of Machinery Industry of the People's Republic of China
Implementation on October 1, 1995
Machinery Industry Standard of the People's Republic of China
Analysis method for hazardous solid wastes from heat treatment salt baths (barium salts, nitrate salts)
1 Subject content and scope of application
JB/T7519-94
This standard specifies the chemical analysis method and allowable deviation range for hazardous solid wastes from heat treatment salt baths (barium salts, nitrate salts). This standard applies to the determination of hazardous solid wastes from heat treatment salt baths.
2 Reference standards
GB5086
Determination of toxicity of barium chloride and sodium nitrite in salt slag leachate; Test method for toxicity of solid waste from non-ferrous metal industry; IB/T6047
Heat treatment salt bath harmless treatment method for hazardous solid waste 3 Determination of fluoride
3.1 Principle
Add excess K, CrO, standard solution to weakly acidic solution to form a precipitate with Ba*. The chemical reaction formula is: K,Cr,O,→2K-+ Cr,O
Cr,O+H,O→2HCrO, 2H-+ 2CrO
Ba* + CrO = BaCrO, +
excess K,Cr,O,. Use ammonium ferrous sulfate standard solution for back titration. Use phenyl-1-aminobenzoic acid (i.e. chromium vanadium indicator) as indicator. The chemical reaction formula is:
2HI,CrO,+6(NH,),Fe(SO,);+ 6H,SO, Cr,(SO,); -+ 3Fe(SO,), + 6(NH,),SO, + 8H,O. The BaCl, content is calculated by the difference in the amount of K,Cr,O, standard solution before and after addition. 3.2 Reagents
The reagents used in this method are of analytical grade (AR) unless otherwise specified; all percentage concentrations, except those specified, are weight volume percentages (W/V)
Potassium dichromate standard solution
Ammonium ferrous sulfate standard solution 0.25M;
Sulfuric acid 1.1 (density 1.84);
Phosphoric acid (density 1.70):
Ammonium benzoate 15%:
Potassium chromate indicator (i.e. phenyl-anthranilic acid indicator) Dissolve 0.27k indicator in 5ml.5% sodium carbonate solution. Dilute to 250ml with water.
3.3 Instruments (or equipment)
In addition to general chemical analysis instruments, it should be equipped with a grinder (or powder machine) and a standard sieve of 20 days/inch or more. 3.4 Samples
3.4.1 Sampling shall be carried out in accordance with Article 1.1 of GB5086. 3.4.2 Sample preparation shall be carried out in accordance with Article 4.1.1 of JB/T6047. Approved by the Ministry of Machinery Industry on October 25, 1994
Implementation on October 1, 1995
Test conditions
See Table 1.
Particle size
Circle-liquid ratio (weight check: water weight)
Protection method
Effluent pH
Precipitant dosagemL
Solution heating temperature
Precipitation standing time
JB/T 7519--94
Water (pH blue 7)
Immerse for more than 20h or heat to boiling for 1~2h or stir for 8h6pH7
0. 05M K,Cr;0;
Note, 1) GB5330-85 <Industrial Metal Wire Mesh Square Hole Net> gives the basic size table of standard sieves with the same hole, such as 0.95mm is equivalent to US 20.8 mesh/inch,
3.5 Analysis steps
Weigh 50g of the sample (dry basis) and place it in a beaker, add 500mL of distilled water, the ring-wave ratio is 1:10, immerse for more than 20 hours (or heat and boil for 1-2 hours), then filter the leaching solution into a 500mL volumetric flask, dilute to the scale with water, and shake well. b. Accurately transfer 20mL of the overflow solution into a 250mL volumetric flask, dilute to the scale with water, and shake well. Pipette 25mL of the diluted solution into a beaker, add 75mL of water and 2mL of ammonium acetate solution, and heat to 50~60C. Accurately insert 20mL of potassium dichromate standard solution, stir thoroughly, and place for 30 minutes or longer. Then, filter with tight filter paper and wash the precipitate with 0.5% ammonium acetate water for 5 to 6 times until the washing water does not appear yellow.
Add 12mL of sulfuric acid (1:1), 2mL of phosphoric acid, and 3 drops of chromium vanadium indicator to the filtrate, and titrate with ammonium ferrous sulfate standard solution until the sample solution changes from purple-red to bright green, which is the end point. Calculate the content of BaCl according to formula (5). (MV/-MV)X0.0694×100
BaCl,% =
Wherein M.-
Molar concentration of potassium dichromate standard solution: dosage of potassium dichromate standard solution, ml.
M.-Molar concentration of ammonium ferrous sulfate standard solution: V.
Amount of ammonium ferrous sulfate standard solution·mL; Sample weight-gt
Number of grams per mole of BaCl.
BaCl (calculated as Ba?-: mg/L) concentration
Wherein: W.-Ba. content.mg
Sample volume, L. bZxz.net
Note: Equivalent concentration-molar concentration> total valence of gold element, 3.6 allowable deviation
.*+(5)
When the concentration of salt slag BaCl, (calculated as Ba*-) is below 1000mg/L, the allowable relative standard deviation is not more than 1.0%. When its concentration is above 1000mg/L, the allowable relative standard deviation is not more than 0.5%. 2
Determination of sodium nitrite
4.1 Principle
JB/T7519-94
In acidic solution, potassium permanganate can oxidize sodium nitrite to sodium nitrate. Its chemical reaction formula is as follows: 2KMnO,+5NaNO,+3H,SO,=2MnSO,+K,SO,+5NaNO,+3H.O The content of sodium nitrite is calculated from the millimoles of potassium permanganate consumed. 4.2 Reagents
Sulfuric acid 11 (density 1.84):
b. Potassium permanganate standard solution 0.1M.
4.3 Instrument (or equipment)
Same as 3.3,
4.4 Test sample
4.4.1 Sampling is the same as 3.4.1.
4.4.2 Sample preparation is the same as 3.4.2
4.4.3 Test conditions are shown in Table 2.
Particle size
Solid-to-liquid ratio (weight of material: weight of water)
Dissolution method
pH of leachate
Amount of oxidant mL
Solution heating temperature C
Oxidation reaction time
4.5 Analysis steps
Water (pH blue)
Soak for more than 20 hours or boil for 1~2 hours or stir for 8h6spH8
0.1 M KMnO, 20
Weigh 50g of the sample (dry basis) and place it in a beaker, add 500mL of distilled water, the solid-to-liquid ratio is 1:10. Soak for more than 20 hours (or boil for 1~2 hours if heated), then filter the leachate into a 500mL volumetric flask, dilute to the scale with water, and shake the hook. b.
Accurately transfer 50mL of the effluent into a 500mL volumetric flask, dilute to the mark with water, shake the hook, accurately pipette 20mL of 0.1M potassium permanganate standard solution into a 300mL conical flask, add 5mL of sulfuric acid (1:1). Spread evenly. After heating to 50-60℃, titrate with the diluted solution until the red color disappears, which is the end point. Calculate the content of NaNO: according to formula (8): NaNO% = 20×M×0. 0345×100
Wherein: M-
—-molar concentration of potassium permanganate standard solution; V
Amount of sample solution, mL;
Number of grams of NaNO, per millimole,
NaNo, (calculated as NO, mg/L) concentration
Wherein: W-—NO: content, mg;
V-sample volume, 1.
Allowable deviation
JB/T7519·94
When the concentration of nitrate stream NaNO, (calculated as NO,) is below 500mg/L, the relative standard deviation is allowed to be no more than 1.05,. Additional remarks:
This standard is proposed and managed by the Mechanical Industry Environmental Protection Technology Research Institute of the Ministry of Machinery Industry. This standard was drafted by the Mechanical Industry Environmental Protection Technology Research Institute, and the main drafters of this standard were Zhang Wenlian and Wu Xinzhong.
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