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should be ascertained visually or by inserting a spatula and laboratories, should be considered suspect if they differ by
scraping the bottom of the container. Continue to shake or stir more than 6.7 % relative.
the sample until specimens are taken for measurement. This 10.2 Bias cannot be determined because there are no ac-
Point is Very Important. cepted standards for nonvolatile content of electrocoat baths.
NONVOLATILE CONTENT INORGANIC PIGMENT CONTENT
8. Procedure
11. Procedure
8.1 Weigh two aluminum dishes separately, each to 0.1 mg
11.1 Place the weighing dishes used for the nonvolatile
and record as W1.
content determination in the muffle furnace at 500°C for 2 h.
8.2 Using a syringe, withdraw 1.0 to 1.5 mL of the well
11.2 After 2 h, remove the dishes from the muffle furnace,
mixed sample, then quickly weigh the syringe to 0.1 mg,
transfer them to a desiccator and allow to cool to room
recording this weight as W2. Transfer the entire contents of the
temperature. After cooling, remove dishes and weigh to 0.1
syringe into the aluminum dish. Reweigh the empty syringe to
mg, recording these weights at W5.
0.1 mg and record as W3. In the case of ultrafiltrate clear liquids
or of low solids paints, increase the specimen size to 5 mL and NOTE 1—If an organic char is still present in the aluminum dish after 2
preheat at 60°C for 2 h. Duplicate this step with the second h in the muffle furnace, continue heating in the furnace until no char is
present.
aluminum dish (8.1).
8.3 Add a few millilitres of water to the specimen in the 12. Calculation
aluminum dishes prior to placing them in the oven. This 12.1 Calculate the percent inorganic pigment as follows:
facilitates uniform spreading of the material. Place the dishes
W5 2 W1
in the 110°C oven for 1 h. % Inorganic Pigment ~ EC Bath! 5 3 100 (2)
W2 2 W3
8.4 Remove the dishes from the oven and allow to cool to
room temperature in a desiccator. Reweigh them to 0.1 mg and where:
record the weights as W4. W1 = weight of empty aluminum dish, g,
W2 = weight of syringe filled with sample, g,
8.5 Retain the dishes for measurement of inorganic pigment W3 = weight of empty syringe, g, and
content as detailed in a following section of these test methods. W5 = weight of aluminum dish and contents after heating in
9. Calculation muffle furnace, g.
9.1 Calculate the percent nonvolatile content as follows: 13. Precision and Bias
W4 2 W1 13.1 Precision estimates are based on an interlaboratory
% NV 5 3 100 (1)
W2 2 W3 study in which the operators in ten different laboratories
analyzed in duplicate on 2 days, four electrocoat bath materials
where:
containing inorganic pigment content ranging from 0.17 to
W1 = weight of empty aluminum dish, g, 4.52 weight %. The results were analyzed statistically in
W2 = weight of syringe filled with sample, g,
accordance with Practice E180. The intralaboratory coefficient
W3 = weight of empty syringe, g, and
W4 = weight of dish and contents after 1 h at 110°C, g. of variation was 2.2 % relative at 40 df and the interlaboratory
coefficient of variation was 10.8 % at 36 df. Based on these
10. Precision and Bias coefficients, the following criteria should be used for judging
10.1 Precision is based on an interlaboratory study in which the acceptability of results at the 95 % confidence level:
the operators in each of ten laboratories analyzed in duplicate 13.1.1 Repeatability—Two results, each the mean of dupli-
on 2 days, four different electrocoat-bath samples with non- cate determinations, obtained by the same operator on different
volatile contents ranging from 0.30 to 25.2 %. The results were days, should be considered suspect if they differ by more than
analyzed statistically in accordance with Practice E180. The 6.3 % relative.
intralaboratory coefficient of variance was 1.6 % at 40 df and 13.1.2 Reproducibility—Two results, each the mean of du-
the interlaboratory coefficient of variation was 2.3 % at 36 df. plicate determinations, obtained by operators in different
Based on these coefficients, the following criteria should be laboratories, should be considered suspect if they differ by
used for judging the acceptability of results at the 95 % more than 31.1 % relative.
confidence level. 13.2 Bias cannot be determined because there are no ac-
10.1.1 Repeatability—Two results, each the mean of dupli- cepted standards for inorganic pigment content of electrocoat
cate determinations obtained by the same operator on different baths.
days, should be considered suspect if they differ by more than
4.6 % relative. 14. Keywords
10.1.2 Reproducibility—Two results, each the mean of du- 14.1 electrocoat bath; muffle furnace; nonvolatile content;
plicate determinations obtained by operators in different pigment content; ultrafiltrates
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