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SY/T 6788-2010: Evaluation procedures of environmental protection for water-soluble oilfield chemicals
SY/T 6788-2010
SY
OIL and GAS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 75-010
E 04
Record No.. 29835-2010
Evaluation procedures of environmental
protection for water-soluble oilfield chemicals
ISSUED ON. AUGUST 27, 2010
IMPLEMENTED ON. DECEMBER 1, 2010
Issued by. National Energy Administration
Table of Contents
Forward ... 3 
1  Scope ... 4 
2  Normative references ... 4 
3  Terms and definitions ... 5 
4  Collection, transport and storage of samples ... 5 
5 Biotoxicity assessment method ... 6 
6  Biodegradability assessment method ... 9 
7  Heavy metal assessment method ... 10 
8  Original record ... 13 
9  Test report ... 13 
Annex A (Normative) Critical value table of correlation coefficient r ... 14 
Annex B (Normative) Test report format of evaluation procedure of
environmental protection for water-soluble oilfield chemicals ... 15 
Test report format of evaluation procedure of environmental protection
for water-soluble oilfield chemicals ... 15 
Bibliography ... 16 
Forward
This Standard shall be used together with SY/T 6787-2010 “Technical requirements for
environmental protection for water-soluble oilfield chemicals”.
Annex A and annex B in this Standard are normative.
This Standard was proposed by and shall be under the jurisdiction of environmental
protection working group of standardization technology committee of petroleum industry.
Drafting organizations of this Standard. CNPC Environmental Inspection Department, and
HSE testing center of environmental technology research institute of china national
petroleum corporation.
Main drafters of this Standard. Li Xiuzhen, Li Jufeng, Li Binlian, Du Weidong, Chen Qin,
Chen Yilong, Li Yuzhong, and Dong Zhihe.
Evaluation procedure of environmental protection for
water-soluble oilfield chemicals
1 Scope
This Standard specifies the environmental protection requirements and evaluation method
of biological toxicity, biodegradability and heavy metal content in water-soluble oilfield
chemicals that are used in oil and gas field.
This Standard applies to the testing and evaluation of biological toxicity, biodegradability
and heavy metal content during the production, purchase and use of water-soluble oilfield
chemicals that are used in oil and gas field.
2 Normative references
The articles contained in the following documents have become part of this Standard when
they are quoted herein. For the dated documents so quoted, all the modifications
(excluding corrections) or revisions made thereafter shall not be applicable to this Standard.
For the undated documents so quoted, the latest editions shall be applicable to this
Standard.
GB/T 6679-2003 General rules for sampling solid chemical products
GB/T 6680-2003 General rules for sampling liquid chemical products
GB 7466-1987 Water quality - Determination of total chromium
GB/T 7468-1987 Water quality - Determination of total mercury - Cold atomic
absorption spectrophotometry
GB/T 7475-1987 Water quality; Determination of copper, zinc, lead and cadmium -
Atomic absorption spectrometry
GB/T 7485-1987 Water quality - Determination of total arsenic - Silver
diethyldithiocarbamate spectrophotometric method
GB 11914-1989 Water quality-Determination of the chemical oxygen demand -
Dichromate method
SY/T 6787-2010 Technical requirements of environmental for water-soluble oilfield
chemicals
product standard.
b) Preparation of samples. take one part of oilfield chemical reagent test solution and
nine part of 30g/L sodium chloride solution according to volume ratio; stir it with
11000r/min±300r/min for 30 minutes; after standing for 60 minutes, calibrate the
concentration of the sample solution to be 106 mg/L. Then sequentially dilute the
solution into sample solutions with different concentrations (105 mg/L, 104
mg/L...10 mg/L and 1mg/L). When the diluted concentration of the measured
sample is close to 50% of the relative luminosity, it is appropriate.
5.2.1.3 Recovery of lyophilized powder microbial inoculums. take an ampoules containing
0.5g of lyophilized powder out of the refrigerator at 2°C~5°C and 2.5g / 100mL sodium
chloride solution. Add 1 mL of cooled 2.5g / 100mL sodium chloride solution into the open
ampoules with lyophilized powder; mix them well. Then place the ampoules with lyophilized
powder in a thermos containing ice cubes. After two minutes, lyophilized powder microbial
inoculums will recover and illuminate; This is recovery bacteria liquid for later use.
5.2.1.4 Preheat and zero-setting of instrument. switch on the bioluminescence photometer;
preheat it for 15 minutes; then set it to zero for use.
5.2.1.5 Inspect the quality of lyophilized powder. take a 2 mL test tube; add 2 mL of 30 g/L
sodium chloride; add 10 µL of recovery bacteria liquid. cover the cork. Shake it upside
down for five times to achieve a uniform. Unplug the cork; put the test tube in test chamber
with bioluminescence photometer to test. If it emits light and shows the number more than
600mV, this bottle of lyophilized powder can be used for test; otherwise, it shall be replaced.
5.2.2 Determination
5.2.2.1 Permutation of test tubes. arrange the test tubes according to the following order
on test tube rack. place the sample test tubes at the front row (referred to as sample tube);
place the control test tubes at the back row (referred to as CK tube). Determine the sample
with the same concentration for three times.
5.2.2.2 Add 30g/L sodium chloride solution. use quantitative liquid bottle to add 2 mL of
30g/L sodium chloride solution in each CK tube.
5.2.2.3 Add sample solution. before test, use 1 mol/L NaOH and 1 mol/L HCl to adjust the
pH value of sample solution to 6.5-8.5. Use 2 mL pipette to add 2 mL of sample solution
into each sample tube.
5.2.2.4 Add recovery bacteria liquid. after the recovery bacteria liquid is stable (about half
an hour), from left to right on test tube rack, in the sequence. sample tube - CK tube -
sample tube - CK tube..., use adjustable micropipette to accurately absorb 10 µL of
recovery bacteria liquid; add it in each tube; cover the cork; shake it upside down for five
times; then remove the cork; put it back to original place. The timing shall be accurate to
second when adding recovery bacteria liquid, which refers to the start time of the reaction
between sample solution and luminescent bacteria liquid. After 15 minutes, record the end
specified in product standard, use distilled water to prepare test solution. Take some
amount of test solution; determine the CODcr of this test solution in accordance with
requirements of GB 11914-1989.
6.2 Determining method of biochemical oxygen demand BOD
According to the determined result of CODcr, determine BOD of this test solution in
accordance with requirements of HJ/T 86-2002.
6.3 Biodegradability assessment method
Determine the index of biodegradability assessment method according to the ratio BOD /
CODcr.
6.4 Test report format
Test report format is shown in annex B.
7 Heavy metal assessment method
7.1 Experiment preparation
7.1.1 Instruments
7.1.1.1 Atomic fluorescence spectrometer.
7.1.1.2 Plasma emission spectrometer.
7.1.1.3 Atomic absorption spectrophotometer.
7.1.1.4 Temperature-control heating plate.
7.1.1.5 Muffle furnace.
7.1.1.6 Glass beads.
7.1.1.7 Quartz crucible.
7.1.2 Reagents
Unless otherwise specified, all reagents shall be analytical reagents that comply with
national standard; test water shall be newly prepared distilled water.
7.1.2.1 Nitric acid (HNO3). ρ20 =1.42g/mL, guarantee reagent.
7.1.2.2 Hydrochloric acid (HCl). ρ20 =1.19g/mL, guarantee reagent.
7.1.2.3 Perchloric acid (HClO4). ρ20 =1.68g/mL, guarantee reagent.
use 1% oxalic acid solution to fix its volume to be 25mL. Shake it well; store it for future
use. In the process of digesting samples, there shall have corresponding standard sample
and reagent blank; the whole process of digestion shall be carried out in
ventilated chamber.
7.2.3 Digestion method of heavy metals - arsenic
Weigh water-soluble oilfield chemical samples (0.1g-0.2g of solid samples and about 1 g
of liquid sample); place it in a PTFE tube. Add 5 mL of 10.1 nitric acid - perchloric acid into
water-moistened solid sample or into liquid sample; shake it well. Cover it with watch glass;
reflux it on electric hot plate at 100°C for one hour. Then rise the temperature to be 120°C
to digest it until there is white smoke. After white smoke is completed, the sample solution
shall be clear or has slight-color, then it is deemed completely digested; otherwise,
continue to add acid to digest it. Take the digested sample out; cool to room temperature.
After adding 10 mL of aqua regia to digest, then add 1 mL of potassium permanganate
solution; place it for 30 minutes after shaking well; then use 1% oxalic acid solution to fix
its volume to be 20mL...