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GB/T 14233.1-1998 (GB/T14233.1-1998)

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GB/T 14233.1-1998: PDF in English (GBT 14233.1-1998)
GB/T 14233.1-1998
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 11.040.20
C 31
Replacing GB/T 14233.1-1993
Infusion, Transfusion, Injection Equipment for Medical
use - Part 1: Chemical Analysis Methods
ISSUED ON: NOVEMBER 26, 1998
IMPLEMENTED ON: FEBRUARY 01, 1999
Issued by: State Bureau of Quality and Technical Supervision
Replaced
Table of Contents
Foreword ... 4
1 Scope ... 6
2 Normative References ... 6
3 General ... 6
Chapter I -- Analysis Method of Dissolution Matter ... 7
4 Preparation of Test Solution ... 7
5 Inspection Items and Analysis Methods ... 8
5.1 Determination of turbidity and color ... 8
5.2 Reducing substances (easy oxides) ... 9
5.3 Chloride ... 12
5.4 pH value ... 13
5.5 Evaporation residue ... 14
5.6 Total content of heavy metal ... 14
5.7 UV absorbance ... 16
5.8 Ammonium ... 16
5.9 Some heavy metal elements ... 17
5.10 Sulfate ... 20
Chapter II -- Analysis Method of Material ... 21
6 Analysis Method of the Total Content of Heavy Metal ... 21
6.1 Principle ... 21
6.2 Preparation of reagents and solutions ... 21
6.3 Preparation of test solution ... 21
6.4 Test procedures ... 22
7 Analysis Method of the contents of some heavy metal elements ... 22
7.1 Atomic absorption spectrophotometer method ... 22
7.2 Colorimetric analysis method ... 22
8 Ignition Residues ... 23
8.1 Test procedures ... 23
8.2 Calculation of results ... 23
Chapter III -- Analysis Method of Ethylene Oxide Residue ... 23
9 Gas Chromatography (Arbitration) ... 23
9.1 Principle ... 23
9.2 Gas chromatograph conditions ... 24
9.3 Preparation of ethylene oxide standard stock solution ... 24
9.4 Specimen preparation ... 24
9.5 Test procedures ... 25
9.6 calculation of results ... 25
10 Colorimetric Analysis Method ... 26
10.1 Principle ... 26
10.2 Preparation of solution ... 26
10.3 Preparation of test solution ... 27
10.4 Test procedures ... 27
10.5 Calculation of result ... 27
Infusion, Transfusion, Injection Equipment for
Medical use - Part 1: Chemical Analysis Methods
1 Scope
This Standard specifies chemical analysis methods of infusion, transfusion, and
injection equipment for medical use.
This Standard is applicable to chemical analysis of infusion, transfusion, injection
equipment for medical use and supporting equipment made of medical polymer
materials. Chemical analysis of other medical polymer products can also use it as a
reference.
2 Normative References
The following standards contain provisions which, through reference in this Standard,
constitute provisions of this Standard. At the time of publication, the editions indicated
are valid. All standards are subject to revision. The parties who are using this Standard
shall explore the possibility of using the latest version of the following standards.
GB 601-1988 Chemical Reagent - Preparations of Standard Volumetric Solutions
GB 602-1988 Chemical Reagent – Preparations of the Formulation and Products
Used in the Test Method
GB 6682-1992 Water for Laboratory Use – Specifications (neq ISO 3696:1987)
People’s Republic of China Pharmacopoeia 2015 Edition
3 General
3.1 All analyses of this Standard are performed in two parallel test groups. The results
shall be within the allowable relative deviation range, and the arithmetic mean value
shall be used as the measurement result. If one is qualified, the other is unqualified,
then the arithmetic mean value shall not be calculated; it shall be re-tested.
3.2 Unless otherwise specified, the reagents used in this Standard are analytically pure.
3.3 If there is no special requirement for test water in this Standard, it shall meet the
requirements of Class-2 water specified in GB 6682.
water; and dilute to 1000mL after cooling.
b) c(KMnO4) = 0.02 mol/L potassium permanganate standard solution: the same as
5.2.1.2d).
c) c(KMnO4) = 0.002 mol/L potassium permanganate standard solution: the same
as 5.2.1.2.e).
d) Starch indicator liquid: take 0.5g of starch and dissolve it in 100mL of water; heat
and boil, then cool off for later-use.
e) c(Na2S2O3) = 0.1 mol/L sodium thiosulfate standard solution: take 26g of sodium
thiosulfate (Na2S2O3 • 5H2O) or 16g of anhydrous sodium thiosulfate; dissolve in
1000mL of water and slowly boil 10 minutes; cool off; add water to 1000mL. After
two weeks, filter it, and calibrate its concentration.
f) c(Na2S2O3) = 0.01 mol / L sodium thiosulfate standard solution: before use, take
0.1mol/L sodium thiosulfate standard solution and dilute it 10 times with freshly
boiled and cooled water.
5.2.2.3 c(Na2S2O3) = calibration of 0.1mol/L sodium thiosulfate solution
Take 0.15g of standard potassium dichromate and dry at 120°C to constant weight;
weigh accurately; place in an iodine volumetric flask; dissolve in 25mL of water; add
2g of potassium iodide and 20mL of dilute sulfuric acid (20% ); shake well; and place
in a dark place for 10min. Add 150mL of water and use the prepared sodium thiosulfate
solution [c(Na2S2O3) = 0.1mol/L] to titrate; add 3mL of starch indicator solution (5 g/L)
near the end point; and continue titration until the solution changes from blue to bright
green. At the same time, a blank test is performed.
5.2.2.4 Test procedures
Take 10mL1) of the test solution prepared in Clause 4; add it to a 250mL iodine
volumetric flask; add 1mL2) of dilute sulfuric acid and 10 mL1) of potassium
permanganate standard solution with the concentration specified in the product
standard; and boil for 3 min; cool quickly; add 0.1g 2) of potassium iodide; stopper and
shake well. Immediately titrate by the sodium thiosulfate standard solution with the
same concentration to the light yellow; add 0.25mL of starch indicator solution; and
continue to titrate by the sodium thiosulfate standard solution to colorless.
Titrate the blank control solution in the same way.
5.2.2.5 Calculation of results
The content of reducing substance (easy oxide) is expressed by the consumed amount
1) 20mL may also be used at the same time.
2) When using 20mL of test solution, add 2mL of dilute sulfuric acid; and 1.0g of potassium iodide.
Take 10mL of sodium chloride standard solution and place it in another 50mL Nessler
colorimetric tube; add 10mL of dilute nitric acid; add water to make it about 40mL; and
shake well to obtain the standard control solution.
Add 1mL of silver nitrate test solution to the above two test tubes; dilute to 50 mL by
water; place them in the dark place for 5min; and observe from above the colorimetric
tube on a black background. Then compare the turbidity between the test solution and
the standard control solution.
If the test solution is colored, unless otherwise specified, two portions of test solutions
may be taken; separately place them into 50mL Nessler colorimetric tubes; and one
portion is added with 1.0mL of silver nitrate test solution; shake well; stand for 10min.
If it is turbid, repeatedly filter it until the filtrate is completely clear; and then add the
standard sodium chloride solution and an appropriate amount of water to make it 50mL;
shake well; and place it in the dark for 5min as a control solution. add 1.0mL of silver
nitrate test solution and an appropriate amount of water to another portion to make it
50mL; shake well, place it in a dark place for 5min; then compare it with the control
solution according to the above method.
5.4 pH value
5.4.1 Method I
Take the test solution and the blank control solution prepared in Clause 4; measure
their pH values with an acidity meter; and use the difference between them as the test
result.
5.4.2 Method II
5.4.2.1 Preparation of solution
a) c(NaOH) = 0.1 mol/L sodium hydroxide standard solution: prepare and calibrate
according to 4.1 of GB 601-1988.
b) c(NaOH) = 0.01 mol/L sodium hydroxide standard solution: take 0.1 mol/L sodium
hydroxide standard solution and dilute with water by 10 times before use.
c) c(HCl) = 0.1 mol/L hydrochloric acid standard solution: prepare and calibrate
according to 4.2 of GB 601-1988.
d) c(HCl) = 0.01 mol/L hydrochloric acid standard solution: take 0.1 mol/L
hydrochloric acid standard solution and dilute it by 10 times with water before
use.
e) Tashiro indicator: dissolve 0.2g of methyl red and 0.1g of methylene blue in
100mL of ethanol [95% (V/V)].
a) Phenolphthalein indicator solution: take 1g of phenolphthalein and add 100mL of
ethanol.
b) Acetate buffer solution (pH 3.5): take 25g of ammonium acetate; add 25 mL of
water to dissolve; add 38mL of hydrochloric acid solution (7 mol/L); and use
hydrochloric acid solution (2 mol/L) or ammonia solution (5 mol/L) accurately
adjust the pH value to 3.5 (indicated by the potentiometric method); and dilute to
100mL by water.
c) Thioacetamide test solution: take 4g of thioacetamide; add water to dissolve it
into 100mL; and store it in the refrigerator. Before use, take 5.0mL of the mixed
solution [consisting of 15mL of sodium hydroxide (1 mol/L), 5.0mL of water and
20mL of glycerol]; add 1.0 mL of the above thioacetamide solution; and heat on
a water bath for 20s; cool and use immediately.
d) Lead standard stock solution: take 0.1598g of lead nitrate dried to constant
weight at 110°C and put it in a 1000mL volumetric flask; add 5mL of nitric acid
and 50mL of water; and dilute to the mark with water after dissolution; and shake
well; and take as the standard stock solution; the lead concentration is 100 µg/mL.
e) Lead standard solution: before use, accurately measure the lead standard stock
solution and dilute it to the required concentration.
5.6.1.3 Test procedures
Take 50mL of the test solution prepared in Clause 4 in a 50mL Nessler colorimeter
tube. Take another 50mL Nessler colorimeter tube; add 1mL of lead standard solution;
and dilute to 50 mL with water. Separately add 2mL of acetate buffer solution (pH 3.5)
to each colorimetric tube; and then separately add 2mL of thioacetamide test solution
each tube; shake well; and stand for 2min. Observe from the top on a white background;
compare the color depth.
5.6.2 Method II
5.6.2.1 Principle
In alkaline solutions, heavy metals such as lead, chromium, copper, and zinc can
interact with sodium sulfide to form insoluble colored sulfides. Take lead as the
representative metal to prepare the standard solution for colorimetry; and the total
content of heavy metals was determined.
5.6.2.2 Solution preparation
a) Sodium hydroxide test solution: take 4.3g of sodium hydroxide and add water to
dissolve it into 100mL.
b) Sodium sulfide test solution: take 1g of sodium sulfide and add water to dissolve
ammonium chloride standard stock solution to the required concentration.
5.8.3 Test procedures
Take 10mL of the test solution prepared in Clause 4 in colorimetric tube with a stopper;
and take another 10mL of ammonium chloride standard solution in another colorimetric
tube. Add 1mL of sodium hydroxide to each of the two tubes and 1 mL of Nessler's
reagent; mix well; after 5min, compare the color depth of the solution in the two
colorimetric tubes.
5.9 Some heavy metal elements
5.9.1 Atomic absorption spectrophotometer method
5.9.1.1 Method summary
Prepare the test solution according to Clause 4; and measure the content of each
element with atomic absorption spectrophotometer.
5.9.1.2 instruments
The atomic absorption spectrophotometer shall be operated according to the
instrument's instruction manual.
5.9.1.3 Analysis method (standard curve method)
Within the recommended concentration range of the instrument, prepare at least 3
standard solutions containing the elements to be measured and their concentrations
are increased in order; and adjust the absorbance of the solvent used to prepare the
standard solution to zero. Then measure the absorbance of each standard solution in
turn; and make a standard curve with respect to the concentration.
Determine the test solution and blank control solution prepared according to Clause 4;
find out the corresponding concentration on the standard curve according to the
absorbance; and calculate the element content.
NOTE: When measuring the content of heavy metals by atomic absorption spectrometry, the
test range can be increased by concentrating the test solution by evaporation. For the
determination of each metal, 2.5 mL of a hydrochloric acid solution with a mass concentration
of ρ(HCl) = 10 g/L was added to 250 mL of the test solution.
5.9.2 Colorimetric analysis method
5.9.2.1 Zinc
5.9.2.1.1 Principle
The reaction between zinc and zinc reagent developed the absorbance at 620nm.
cs – concentration of heavy metal corresponding to the test solution, in µg/mL;
cr – concentration of heavy metal corresponding to the standard control solution, in
µg/mL;
As – absorbance of the test solution;
At – absorbance of the standard control solution.
5.9.2.2 Lead
5.9.2.2.1 Principle
Lead ions form a red complex with dithizone chloroform solution under weak alkaline
(pH 8.6~11) conditions.
5.9.2.2.2 Preparation of reagents and solutions
a) 0.1% dithizone chloroform stock solution: take 0.10g of dithizone and dissolve in
chloroform; dilute to 100mL; store in brown bottle; and then place in refrigerator.
If dithizone is not pure, it can be purified by the following method: take 0.20g of
dithizone; dissolve it in 100mL of chloroform; filter it in a 250mL funnel through
absorbent cotton; and use 20mL of 3% (V/V) ammonia to repeatedly extracted
for several times until the chloroform phase is almost green. Merge water phase
into another separatory funnel and wash the water phase twice with 10mL of
chloroform each time. The chloroform phase was discarded; and the water phase
was acidified by 10% (V/V) sulfuric acid to separate out the dithizone; and then
extract twice by 100mL of chloroform each time. The chloroform phases were
combined and poured into a brown bottle.
b) Dithizone chloroform solution with absorbance of 0.15 (transmittance of 70%):
before use, take an appropriate amount of dithizone chloroform stock solution
and dilute with chloroform to an absorbance of 0.15 (wavelength 510nm, 1cm
cuvette).
c) Phenol red indicator solution: take 0.1g of phenol red and dissolve it in 100mL of
ethanol.
d) 50% ammonium citrate solution: take 50g of ammonium citrate and dissolve it in
100mL of water; take phenol red as an indicator; alkalize it by ammonia water
(pH 8.5~9); extract by the dithizone stock solution; 20mL each time, until
dithizone turns green. The chloroform layer was discarded, and the water layer
was washed by chloroform for several times; 25mL each time, until the
chloroform layer was colorless. The chloroform layer was discarded and the
water layer was taken.
and dilute to 100mL.
d) Acetic acid solution (300 g/L): take 30mL of glacial acetic acid; add 100mL of
water; and shake well.
5.10.2 Test procedures
Pipette 0.75mL of 95% ethanol solution into a colorimetric tube with a stopper; add
0.5mL of barium chloride solution and 0.25mL of acetic acid solution; add 1.5mL of
sulfate standard solution under continuous shaking conditions; and mix then shake for
30s; take 15mL of test solution; and add 0.3mL of acetic acid solution to acidify. This
acidified solution was added to the above mixture.
Use 15mL of sulfate standard solution with the mass concentration ρ(SO42-) = 10 mg/L;
prepare the control suspension in the same way.
Check after 5 min, the suspension must not be more turbid than the control solution.
Chapter II -- Analysis Method of Material
6 Analysis Method of the Total Content of Heavy Metal
6.1 Principle
In weakly acidic solutions, heavy metals such as lead, cadmium, copper, and zinc can
interact with thioacetamide to form insoluble colored sulfides. Use lead standard
solution as a standard for colorimetry to determine their total content.
6.2 Preparation of reagents and solutions
Performed as described in 5.6.1.2.
6.3 Preparation of test solution
Take 2g of sample and cut it into 5mm×5mm pieces; put them into a porcelain crucible;
slowly heat to carbonize; add 2mL of nitric acid and 5 drops of sulfuric acid after cooling;
and heat until the white smoke disappears. Burn at 500°C~550°C to make them ash;
after cooling, add 2mL of hydrochloric acid; and place on a water bath and evaporate
to dryness; add 3 drops of hydrochloric acid to wet the residue; add 10mL of water;
heat for 2 minutes; add a drop of phenolphthalein test solution; and then add ammonia
test solution until the above solution turns reddish. Add 2mL of acetate buffer solution
(pH 3.5) (if turbid, filter, and wash the precipitate with 10mL of water); transfer the
solution into a 50mL volumetric flask; and add water to make a 50mL test solution.
Place another porcelain crucible with 2mL of nitric acid, 5 drops of sulfuric acid and
2mL of hydrochloric acid on a water bath to evaporate to dryness; and then wet the
residue with 3 drops of hydrochloric acid. The following operations are the same as the
preparation method of the test solution, making it a blank control solution.
6.4 Test procedures
Take 50mL of the test solution and add it to a 50mL Nessler colorimetric tube. Add
another 1mL of lead standard solution to another 50mL Nessler colorimetric tube and
add the blank control solution to 50mL. Separately add 2mL of thioacetamide test
solution to each of the two colorimetric tubes; shake well; and stand for 2min. Observe
from above on a white background, compare the color depth.
7 Analysis Method of the contents of some heavy metal
elements
7.1 Atomic absorption spectrophotometer method
7.1.1 Method summary
The test solution was prepared according to 6.3, and the content of each element was
measured by atomic absorption spectrophotometer.
7.1.2 Instrument
The atomic absorption spectrophotometer shall be operated according to the
instrument's instruction manual.
7.1.3 Analysis method (standard curve method)
Within the recommended concentration range of the instrument, prepare at least 3
standard solutions containing the elements to be measured and their concentrations
are increased in order; and adjust the absorbance of the solvent used to prepare the
standard solution to zero. Then measure the absorbance of each standard solution in
turn, and make a standard curve with respect to the concentration.
Determine the test solution and blank control solution prepared according to 6.3; find
out the corresponding concentration on the standard curve according to the
absorbance; and calculate the content of the element.
7.2 Colorimetric analysis method
7.2.1 Zinc
Prepare the test solution and blank control solution according to 6.3 and perform
9.4.2 Cut the sample into 5mm long pieces; take 2.0g of it into the extraction container;
add 10mL of water; keep 40mL of head space. The pressure in the container is normal
pressure; and place in a constant temperature water bath at 60°C±1°C for 20min.
9.5 Test procedures
9.5.1 Use the stock solution to prepare a standard solution with six series
concentrations of 1×10-3 g/L ~ 1×10-2 g/L. Separately take 10mL each and process
according to 9.4.2.
Use a glass syringe to quickly take 1mL of the upper gas from the equilibrated standard
sample and specimen in order; and inject it into the injector; and record the peak height
(or area) of ethylene oxide.
NOTE 1: Use one person as much as possible in one analysis and use the same 1mL glass
syringe;
NOTE 2: The syringe is made the same constant temperature as the sample in advance;
NOTE 3: Pay attention to the change in the retention time of ethylene oxide every time to
prevent gas leakage from the injection vaporization pad;
NOTE 4: Each sample (including the standard sample) is analyzed for three times in the
shortest time as much as possible. Two of the three analyses must have a difference of no
more than 5%, otherwise the sample shall be reanalyzed.
9.5.2 Use the measured data of the standard sample to draw a standard curve (X: EO
concentration, g/L; Y: peak height or area).
9.5.3 Find out the corresponding concentration of the sample from the standard curve.
If the measured sample results are not in the range of the standard curve, the
concentration of the standard solution shall be changed and the standard curve re-
created.
9.6 calculation of results
The residual amount of ethylene oxide is expressed by an absolute content or a relative
content.
9.6.1 Calculate the absolute content of ethylene oxide in the sample according to
Formula (6):
Where:
WEO – absolute content of ethylene oxide per unit product, in mg;
......
 
(Above excerpt was released on 2020-03-31, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT14233.1-1998