Designation: D7191 − 10

Standard Test Method for

Determination of Moisture in Plastics by Relative Humidity
Sensor1
This standard is issued under the fixed designation D7191; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3. Terminology
1.1 This test method covers the quantitative determination 3.1 Definitions—The definitions used in this test method are
of water down to 20 ppm in plastics using a relative humidity in accordance with Terminology D883.
sensor.
4. Summary of Test Method
1.2 Values stated in SI units are to be regarded as standard. 4.1 A sample is loaded into a septum-capped glass vial that
1.3 Specimens tested in this test method can reach or exceed is moved into a heater to evolve the volatiles from the sample
250°C, use caution when handling them after testing has into the headspace. A coaxial needle, or two needle set, pierces
completed. the septum of the vial as it enters the heater. A dry carrier gas
1.4 This standard does not purport to address all of the then flows into the vial and carries the evolved volatiles in the
safety concerns, if any, associated with its use. It is the headspace into the sensor manifold. In the sensor manifold, the
responsibility of the user of this standard to establish appro- carrier gas is cooled to allow high-boiling volatiles to condense
priate safety and health practices and determine the applica- on a hydrophobic filter. The filter’s hydrophobic properties
bility of regulatory limitations prior to use. allow the moisture in the carrier gas to pass through and then
be measured as an increase in potential at the relative humidity
NOTE 1—There is no known ISO equivalent to this standard. sensor. This sensor signal is integrated over time to provide a
measurement of the total mass of water in the sample. The total
2. Referenced Documents
moisture is then divided by sample mass to yield moisture
2.1 ASTM Standards:2 content.
D1193 Specification for Reagent Water 4.2 This test method utilizes a sealed, airtight flow system
D883 Terminology Relating to Plastics that prevents contamination of the analyzer from water present
D1600 Terminology for Abbreviated Terms Relating to Plas- in the atmosphere.
tics
D6869 Test Method for Coulometric and Volumetric Deter- 5. Significance and Use
mination of Moisture in Plastics Using the Karl Fischer 5.1 This test method is intended for use as a control,
Reaction (the Reaction of Iodine with Water) acceptance, and assessment test.
E177 Practice for Use of the Terms Precision and Bias in 5.2 Moisture can seriously affect the processability of plas-
ASTM Test Methods tics. It is possible that high moisture content will cause surface
E691 Practice for Conducting an Interlaboratory Study to imperfections (that is, splay or bubbling) or degradation by
Determine the Precision of a Test Method hydrolysis. Low moisture (with high temperature) has been
known to cause solid phase polymerization.
1
5.3 The physical properties of some plastics are greatly
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. affected by the moisture content.
Current edition approved April 1, 2010. Published June 2010. Originally
approved in 2005. Last previous edition approved in 2005 as D7191 - 05.
6. Interferences
DOI:10.1520/D7191-10.
2
6.1 Elevated concentrations of some common solvents such
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
as methanol, ethanol and acetone will give biased high read-
Standards volume information, refer to the standard’s Document Summary page on ings due to their polar characteristics and ability to permeate
the ASTM website. the thermoset polymer layers of the relative humidity sensor.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D7191 − 10
7. Apparatus 9.2 Due to the hygroscopic nature of many plastics, samples
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7.1 Moisture Analyzer , an apparatus that consists of: shall be stored in airtight containers made of glass or other
7.1.1 Flow Regulator, capable of maintaining the carrier gas qualified or suitable material.
flow rate within the manufacturer’s specified conditions. 9.3 Samples that have been heated to remove moisture prior
7.1.2 Flow Meter, capable of measuring the carrier gas flow to processing and testing shall be allowed to cool to room
rate in accordance with the manufacturer’s specified condi- temperature in a sealed container prior to determination.
tions. 9.4 Test specimens in the form of liquid, powders, pellets, or
7.1.3 Manifold, which provides: ground material.
7.1.3.1 A thermally stable port for mounting and operation
of the relative humidity sensor. 10. Calibration and Standardization
7.1.3.2 Inlet and outlet ports for the carrier gas. 10.1 To maintain the integrity of the test results, the vial
7.1.3.3 A cold trap filter loop which filters out particulates heater shall be calibrated using a NIST-traceable temperature
and re-condensed high boiling volatiles. calibration interface, and the RH sensor shall be verified and
7.1.3.4 A port for mounting the coaxial needle, or two calibrated using NIST-traceable capillary tubes. Alternatively,
needle set. other suitable instrument calibration methods and standards
7.1.4 Coaxial Needle, a needle which has a dual flow path can be used as specified by the instrument manufacturer.
allowing the carrier gas to flow into the sample vial and then
back into the manifold, or a two needle set configured to allow 10.2 Perform the vial heater calibration in accordance with
inflow into the sample vial through one needle and outflow the manufacturer’s instructions.
from the sample vial through the second needle. 10.3 If the results are not within the acceptable range,
7.1.5 Relative Humidity (RH) Sensor, a capacitive sensing contact the analyzer manufacturer.
element that measures the relative humidity of the carrier gas 10.4 Perform the RH sensor verification daily in accordance
coming into the manifold. with the manufacturer’s instructions by way of using a capil-
7.1.6 Sample Vial Heater, capable of maintaining the sample lary tube (see 8.1) filled with water (see 8.4) or other method
vial temperature within 1°C of the programmed temperature as specified by the instrument manufacturer.
between 25°C and 275°C.
7.1.7 Microcontroller, which provides: 10.5 If the RH sensor verification result is not within the
7.1.7.1 Capability of integrating and converting the RH acceptable range, perform the RH sensor calibration in accor-
sensor signal. dance with the manufacturer’s instructions using a capillary
7.1.7.2 Capability of controlling the temperature of the tube (see 8.1) filled with water (see 8.4) or other method as
sample vial heater and sensor manifold. specified by the instrument manufacturer.
7.2 Balance, external, with 1-mg readability. 10.6 Repeat step 10.4 to verify RH sensor calibration.
10.7 If results are not within the acceptable range, contact
8. Reagents and Materials the analyzer manufacturer.
8.1 Capillary Tubes—NIST-traceable at the desired total 11. Procedure
mass of water, typically 1000 µg, or other qualified water
standard devices. 11.1 Sample Analysis:
11.1.1 Turn on the analyzer.
8.2 Sample Vials—70-mm tall and 25-mL capacity. 11.1.2 Establish carrier gas flow in accordance with the
8.3 Sample Vial Septa—polytetrafluoroethylene (PTFE)- manufacturer’s specifications.
coated silicone. 11.1.3 Program the analyzer with the appropriate test con-
8.4 Water—Unless otherwise indicated, references to water ditions.
shall be understood to mean reagent water as defined by Type NOTE 2—Suggested test conditions are listed in Appendix X1. If test
II of Specification D1193. conditions for a specific material are not listed in Appendix X1, they will
have to be determined experimentally as described in Appendix X2 or by
8.5 Carrier Gas—Any dry gas with water content less than contacting the analyzer manufacturer.
3 ppm including but not limited to dry air, nitrogen, helium or
11.1.4 Place a clean vial on the balance and tare it.
argon.
11.1.5 Refer to Table X2.1 and place the appropriate amount
of sample in the vial keeping in mind that the vial must remain
9. Sampling and Test Specs and Units
less than half full.
9.1 Due to the small specimen size, exercise care to ensure 11.1.6 Place the vial with sample back on the balance and
that the specimen is representative of the sample. reweigh.
11.1.7 Record the sample weight.
11.1.8 Cap the vial ensuring the PTFE-coated side of the
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The sole source of supply of the apparatus known to the committee at this time septum is facing the inside of the vial.
is Arizona Instrument, 1912 West 4th Street, Tempe, AZ 85281. If you are aware of
alternative suppliers, please provide this information to ASTM International
11.1.9 With the vial on its side, ensure the sample is evenly
Headquarters. Your comments will receive careful consideration at a meeting of the distributed in the vial.
responsible technical committee,1 which you may attend. 11.1.10 Place the vial in the testing position in the analyzer.

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 D7191 − 10
TABLE 1 Moisture in Plastics by Relative Humidity Sensor (%)
Material Average Repeatability Reproducibility Repeatability As % of Avg. Reproducibility As % of Avg.
Standard Standard Limit Limit
Deviation Deviation
x Sr SR r r R R
Polycarbonate 0.09059 0.00487 0.02240 0.01364 15.05 0.06272 69.23
Polypropylene 0.01025 0.00149 0.00587 0.00418 40.80 0.01642 160.2
Nylon 6 0.42595 0.01702 0.05677 0.04764 11.19 0.15894 37.32
ABS 0.26304 0.00617 0.02333 0.01729 6.57 0.06533 24.84

11.1.11 Begin the program and follow the prompts for 14. Precision and Bias
starting the analysis.
14.1 The precision of this test method is based on an
11.1.12 At the end of the test, the bottle will be very hot so
interlaboratory study of D7191 - 05 conducted in 2009. Twelve
use caution when handling.
laboratories tested a total of four different materials. Every test
11.1.13 Record the result as displayed.
result represents an individual determination. Each laboratory
11.1.14 Repeat steps 11.1.4-11.1.14 for subsequent tests.
reported triplicate test results. Practice E691 was followed for
12. Calculation or Interpretation of Results the design and analysis of the data.
12.1 If results are displayed in total micrograms (µg) of 14.1.1 Repeatability limit (r)—Two test results obtained
water present, then calculate percent moisture content of the within one laboratory shall be judged not equivalent if they
sample as follows: differ by more than the r value for that material; r is the interval
representing the critical difference between two test results for
Moisture content, % 5 R 3 10^24/W (1)
the same material, obtained by the same operator using the
where: same equipment on the same day in the same laboratory.
R 5 total water result for sample, mg, and 14.1.1.1 Repeatability limits are listed in Table 1.
W 5 sample weight, g. 14.1.2 Reproducibility limit (R)—Two test results shall be
12.2 If results are displayed as percent of water present and judged not equivalent if they differ by more than the R value
conversion to parts per million (PPM) is desired, calculate as for that material; R is the interval representing the critical
follows: difference between two test results for the same material,
obtained by different operators using different equipment in
PPM 5 Moisture content ~ % ! 3 10,000 (2)
different laboratories.
12.3 No further calculation or interpretation is necessary. 14.1.2.1 Reproducibility limits are listed in Table 1.
13. Report 14.1.3 The above terms (repeatability limit and reproduc-
ibility limit) are used as specified in Practice E177.
13.1 Report the following information:
13.1.1 Complete identification of the sample tested, includ- 14.1.4 Any judgment in accordance with statements 14.1.1
ing type of material, source, and manufacturer’s code, and 14.1.2 would have an approximate 95 % probability of
13.1.2 Date of test, being correct.
13.1.3 Individual specimen size,
13.1.4 Individual specimen moisture, and 15. Keywords
13.1.5 Average moisture. 15.1 moisture determination; plastics

APPENDIXES

(Nonmandatory Information)

X1. MOISTURE ANALYZER

X1.1 Suggested test conditions for selected plastics are not intended to be inclusive of every grade of every plastic and it will
given in Table X1.1. potentially be necessary to contact the analyzer manufacturer for assis-
NOTE X1.1—These suggested conditions were determined through tance with determining the best test conditions for your specific material.
extensive tests that have been completed on these common plastics. It is

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 D7191 − 10
TABLE X1.1 Suggested Test Conditions for Selected Plastics
Material Test Temp (°C) Ending Criteria (µg/s) Sample Size (g) Vial Purge (s)
ABS 230 Rate = 0.75 1-2 45
ABS + PC 200 Predict 5-7 45
EVOH 215 Rate = 0.75 1-2 45
POM 150 Predict 2-3 45
PA 6 200 Predict 1-2 45
PA 6/6 230 Rate = 0.75 1-2 45
PBT 230 Predict 5-7 45
PC 230 Rate = 0.75 5-7 45
PEI 230 Rate = 0.50 3-5 45
PET 215 Rate = 0.50 5-7 45
PS 250 Rate = 0.75 2-3 45
PVC 200 Rate = 0.50 3-5 45
TPE 200 Predict 3-5 45
TPU 230 Predict 1-2 45

X2. DETERMINING OPTIMAL TEST CONDITIONS

TABLE X2.1 Recommended Sample Sizes than half full to prevent the sample coming in contact with the
Expected Moisture, % Recommended Sample coaxial needle during testing.
Size, g
Less than 0.01 6.9-7.1 X2.1.2 Test Temperature—Start at a temperature 20°C be-
0.01-0.03 4.9-5.1 low the melting or decomposition temperature of the material,
0.03-0.05 2.9-3.1
0.05-0.15 0.9-1.1
or both. Increase or decrease the temperature in increments of
Greater than 0.15 0.4-0.6 5°C to achieve the desired results. If no significant change in
the test result occurs, proceed to rate adjustment for further
optimization.
X2.1 When determining the optimal test conditions for a X2.1.3 Ending Criteria—Start at a rate of 0.50 µg/s. In-
material, it is useful to have a Karl Fischer apparatus available crease or decrease the rate in increments of 0.05 µg/s to achieve
and test in accordance with Test Method D6869. Optimization the desired result.
of test conditions may include adjustment of the sample size, X2.1.4 Vial Purge Time—Increase or decrease the vial
test temperature, ending criteria or vial purge. Use the follow- purge time as needed to minimize interferences from atmo-
ing guidelines for optimizing test conditions: spheric moisture present in the sample vial or the presence of
X2.1.1 Sample Size—Increase or decrease the sample size low boiling volatiles present in the sample. It will also be
as needed to produce a result where the total mass of water necessary to decrease the vial purge in some cases to zero when
present is ~1000 µg. See Table X2.1 for recommended sample testing materials with high moisture content or where the
sizes keeping in mind that the sample vial must remain less moisture evolves quickly.

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