中华人民共和国国家标准

黄药化学分祈方法 UDC 622. 765

. 06 : 543. 06
乙酸铅滴定法测定黄原酸盐含量
GB 8 1 5 0. 1 -
Methods for chemical analysis of xanthates 87
The lead-acetate titration method for determination of xanthate content

The lead-acetate titration method for determination of xanthate content

1. The priciple:
This method is suitable to test the xanthate content in Sodium series Xanthate and Potassium series Xanthate of
Ethyl, Isopropyl, Butyl, Isobutyl, Amyl and other low- carbon alkyl. The indicator is Sodium Nitroprusside,
potassium ferricyanide is used for oxidizing the alkali metal sulfides and other impurity to free sulfide, in order
to eliminate the interference of these items. The chemical reaction is :
S2- +2[Fe(CN)6]3- →S↓+2[Fe(CN)6]4-
The rhodizonic acid sodium salt is indicator, the lead acetate standard solution is titrated to xanthate, the
chemical reaction is as follows:
2ROCSS-+Pb2+→(ROCSS)2Pb↓
2, The reagent:
◆ Hydrochloric acid (Gravity 1.19)
◆ Hydrochloric acid(6N)
◆ Glacial acetic acid
◆ Aqua ammonia (10%)
◆ Ammonia-Ammonium chloride buffer solution: Prepare according to Article 38 Item (1) of GB 603---77
《Preparations of Reagent Solutions》
◆ Hexamethylenetetramine-Hydrochloric acid buffer solution: put 300g Hexamethylenetetramine into 500ml
water, add 30ml hydrochloric acid (gravity 1.19), and then add some water to dilute to 1000ml
♦Potassium ferricyanide solution(1%), be stored in bronze bottles, prepare when using
◆ Eriochrome black T indicator solution(0.5%), weigh 0.5g eriochrome black T and 2g hydroxylamine
hydrochloride, then be soluble in 100ml alcohol, prepare when using.
◆ Xylenol Orange indicator solution: (0.2%)
◆ Sodium Nitroprusside indicator solution(2%): prepare when using
◆ Rhodizonic acid sodium salt indicator solution(0.1%): prepare when using
◆ Ammonium chloride
◆ Zinc oxide: standard reagent
◆ Lead acetate
◆ Disodium ethylene diamine tetraacetate standard solution(0.0125M)

Prepare： put 5g EDTA disodium salt dehydrate heated to be soluble in water, cool and shake. Calibration:

weigh 1.0000g zinc oxide ( standard reagent) which is burned to constant weight in 800℃, moisturize it with

little water, and add 5ml hydrochloric acid(6N), until zinc oxide be soluble, move it to the 500ml measuring

flask, then dilute to the mark in the flask and shake. Put 30.00~35.00ml solution, add 20ml water, add in 10%

aqua ammonia to neutralize it to PH7~8. And add 10ml Ammonia-Ammonium chloride buffer solution, 5

drops eriochrome black T indicator, titrate the solution from purple to pure blue by EDTA standard solution, do

the blank test

GB8150.1-87 中国有色金属工业总公司 1987-01-27批准

 at the same time.

Calculate: Molar concentration(M) of EDTA standard solution is calculated as follows:

G
M
(V1 - V2 )x0.08138

In the formula:

G -------- weight of zinc oxide, g

V1---------volume of EDTA standard solution, ml

V2 -------- volume of EDTA standard solution in the blank test, ml

0.08138 ------ the grams of zinc oxide in mol/ml

◆ Lead acetate standard solution (0.025N)

Prepare: put 4.75g lead acetate [ Pb(C2H3O2)23H2O] to be soluble in 500ml water, add 6ml

glacial acetic acid, dilute with water to 1000ml, shake.

Calibration: put exactly 30.00~35.00ml lead acetate standard solution in the beaker, then add 30ml

water and 10ml hexamethylenetetramine buffer solution, add more 5 drops Xylenol Orange

indicator solution, until titrate it to yellow by using the given concentration EDTA standard

solution.

Calculate: Equivalent concentration N of lead acetate standard solution is calculated as follows:

2xV1xM
N
V2

In the formula:

V1 ---------the consumption of EDTA standard solution in the titration, ml;

M --------- Molar concentration of EDTA standard solution

V2 --- take out the standard solution of the lead acetate , ml

2 -- 1 Mole's EDTA equivalent to equivalent number of acetic lead
Calibration 3 copies, the range should not more than 0.00005N
3. Analysis steps:
(1) With distilled water or deionized water analysis
(2) The xanthate samples preservation conditions: Moisture proof and prevent heat、Cap tight. Try
to shorten the time of opened the lid when analysis.
（3）Use the weighing bottle which is with cap to take about 10g sample . move them all to the

GB8150.1-87 中国有色金属工业总公司 1987-01-27批准

 500 milliliter battle. Dilution to the scale, shake up and then accurate take 5.00 ml to the 250 ml
beaker. Plus 2 drops of the nitro iron sodium cyaniding indicator, if sample contains alkaline metal
sulfides impurities, Solution is violet, Now constantly shake a beaker, Drop join by the potassium
ferricyanide, until the violet solution disappear, then ecessive add 1 drop to ensure that the
oxidation completely. If the potassium ferricyanide addition amount more than 1 ml, then need to
take another 5 ml sample solution into 250 ml beaker. Join about 0.2 g chloride, remove the
sulfide impurities according to the above operation, add 100 ml water into the beaker, under the
stir with acetic lead solution titration, near the finish add 1-2 ml of rosy acid sodium indicator, and
continue the titration until the meat red suddenly appeared to end.
4. Analysis results of calculation
Calculate the percentage content of xanthenes according to formula following:
Xanthenes content (%) = {(N*V*M/1000)/5*W/500}*100
In the formula:
N- Acetic gram-equivalent weight concentration of lead standard solution
V- Consumption of acetic acid lead standard solution when titration, ml
M- Molecular weight of the xanthenes
W- Says take sample weight, g
Several common xanthenes, molecular weight as below:
SEX: 144.2
SIPX: 158.2
SIBX: 172.3
SIAX: 186.3
PIAX: 202.3
5. Admissible error
This method allows the average poor must not be more than 5% determination
Acetic titration free alkali content
1. Principle:
Use the impurities carbonate in the barium chloride and xanthenes generating precipitation,
eliminate interference, with phenolphthalein for indicator. Use acetic acid standard solution to
titration the free alkali in the xanthenes.
2. Reagent
(1) Barium chloride solution (10%)
(2) Phenolphthalein batch reagent solution (1%), take 1 gram phenolphthalein soluble in 20 ml of
alcohol, diluted to 100 ml
(3) Acetic acid standard solution (0.05N):according to the prescribed method in the①②of second
part article 1 of GB60-77《Standard solution method of preparation 》to configuration and
calibration
3. Analysis steps ：
From this sample of xanthenes which is preparation use this method for determining xanthenes
content, place 50 ml into the 250 milliliter cone-shaped bottle, add 10ml barium chloride solution,
then add two to three drops of phenolphthalein indicator, titration with acetic acid standard
solution, titrate speed slightly faster when close to the end, always drops to pink disappear 30
seconds end doesn't return.
4. Analysis results of computation

GB8150.1-87 中国有色金属工业总公司 1987-01-27批准

 Calculate the percentage content of free alkali according to formula following:
Free alkali (%) = {(N*V*40/1000)/(50*w/500)}*100
In the formula:
N- The equivalent concentration acetic acid standard solution ;
V-Consumption acetic acid standard solution when titration, ml;
W- Says take sample weight, g;
40- Gram-equivalent weight of sodium hydroxide (if analysis the potassium xanthenes, the gram-
equivalent weight of potassium hydroxide should be 56.1)
5. Admissible error
This method allows the average poor must not be more than 0.02% determination

GB8150.1-87 中国有色金属工业总公司 1987-01-27批准