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erah
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da. Pada titik akhir titrasi dengan EDTA, indikator akan lepas kembali dan larut
an menjadi
\par}{\phpg\posx2118\pvpg\posy10455\absw8971\absh1063 \sl-237 \f10 \fs18 \cf0 be
rwarna ungu. \par
}
{\phpg\posx2118\pvpg\posy11883\absw342\absh636 \b \f10 \fs18 \cf0 \b \f10 \fs18
\cf0 3.2
\par}{\phpg\posx2118\pvpg\posy11883\absw342\absh636 \sl-238 \par\b \f10 \fs18 \c
f0 {\b0 a) }\par
}
{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \b \f10 \fs18 \cf0 \fi53 \b \f1
0 \fs18 \cf0 Bahan
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-168 \par\par\b \f10 \f
s18 \cf0 \fi68 {\b0 Indikator}{\b0 mureksid}{\b0 (C }{\b0\dn006 \fs11 8}{\b0
H }{\b0\dn006 \fs11 8}{\b0 N }{\b0\dn006 \fs11 6}{\b0 O }{\b0\dn006 \fs11 6}{
\b0 ) }
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-223 \par\b \f10 \fs18
\cf0 {\b0 1)}{\b0
Timbang}{\b0 200}{\b0 mg}{\b0 mureksid}{\b0 dan}{\b
0 100}{\b0 g}{\b0 kristal}{\b0 natrium}{\b0 klorida}{\b0 (NaCl),}{\b
0 kemudian }
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-237 \b \f10 \fs18 \cf0
\fi334 {\b0 dicampur. }
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-313 \b \f10 \fs18 \cf0
{\b0 2)}{\b0
Gerus}{\b0 campuran}{\b0 tersebut}{\b0 hingga}{\b0 memp
unyai}{\b0 ukuran}{\b0 40}{\b0 mesh}{\b0 sampai}{\b0 dengan}{\b0 50
}
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-237 \b \f10 \fs18 \cf0
\fi334 {\b0 mesh. }
\par}{\phpg\posx2583\pvpg\posy11883\absw8512\absh2057 \sl-314 \b \f10 \fs18 \cf0
{\b0 3)}{\b0
Simpan}{\b0 dalam}{\b0 botol}{\b0 yang}{\b0 tertutup}{\b0
rapat. }\par
}
{\phpg\posx6057\pvpg\posy14932\absw694\absh189 \b \f10 \fs17 \cf0 \b \f10 \fs17
\cf0 1 dari 8 \par
}
\sect\sectd\pard\plain
\pgwsxn12240\pghsxn15840
{\phpg\posx2118\pvpg\posy806\absw2082\absh207 \b \f10 \fs18 \cf0 \b \f10 \fs18 \
cf0 SNI 06-6989.13-2004 \par
}
{\phpg\posx2118\pvpg\posy1607\absw228\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 b)
\par
}
{\phpg\posx2118\pvpg\posy3498\absw228\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 c)
\par
}
{\phpg\posx2118\pvpg\posy4764\absw228\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 d)
\par
}
{\phpg\posx2651\pvpg\posy1607\absw8446\absh11397 \f10 \fs18 \cf0 \f10 \fs18 \cf0
Indikator Eriochrome Black T (EBT = C {\dn006 \fs11 20}H{\dn006 \fs11 12}N {\
an
\par}{\phpg\posx2118\pvpg\posy5466\absw8969\absh2272 \sl-237 \f10 \fs18 \cf0 \fi
319 ke dalam labu Erlenmeyer 250 mL.
\par}{\phpg\posx2118\pvpg\posy5466\absw8969\absh2272 \sl-171 \par\f10 \fs18 \cf0
b) Apabila tidak dapat segera dianalisis, awetkan contoh uji dengan H
NO{\dn006 \fs11 3} sampai pH 2. \par
}
{\phpg\posx2118\pvpg\posy7920\absw5917\absh490 \f10 \fs18 \cf0 \fi319 \f10 \fs18
\cf0 Waktu simpan contoh uji tidak lebih dari 6 bulan.
\par}{\phpg\posx2118\pvpg\posy7920\absw5917\absh490 \sl-314 \f10 \fs18 \cf0 c)
Perlakuan awal ({\i pre}{\i treatment}) contoh uji atau limbah cair \par
}
{\phpg\posx2456\pvpg\posy8546\absw8586\absh502 \f10 \fs18 \cf0 \f10 \fs18 \cf0 J
ika contoh uji memerlukan digesti awal, lakukan digesti dengan asam nitrat (HNO{
\dn006 \fs11 3}) atau
\par}{\phpg\posx2456\pvpg\posy8546\absw8586\absh502 \sl-237 \f10 \fs18 \cf0 deng
an asam nitrat - asam perklorat - asam fluorida (HNO {\dn006 \fs11 3} - HClO{\d
n006 \fs11 4} - HF), dengan cara \par
}
{\phpg\posx2456\pvpg\posy9023\absw3105\absh674 \f10 \fs18 \cf0 \f10 \fs18 \cf0 s
ebagai berikut:
\par}{\phpg\posx2456\pvpg\posy9023\absw3105\absh674 \sl-252 \par\f10 \fs18 \cf0
{\b 1)}{\b
Digesti}{\b asam}{\b nitrat}{\b (HNO}{\b\dn006 \fs11 3}{\b ) }
\par
}
{\phpg\posx2795\pvpg\posy9812\absw308\absh1481 \f10 \fs18 \cf0 \f10 \fs18 \cf0 (
a)
\par}{\phpg\posx2795\pvpg\posy9812\absw308\absh1481 \sl-275 \par\f10 \fs18 \cf0
(b)
\par}{\phpg\posx2795\pvpg\posy9812\absw308\absh1481 \sl-314 \f10 \fs18 \cf0 (c)
\par}{\phpg\posx2795\pvpg\posy9812\absw308\absh1481 \sl-275 \par\f10 \fs18 \cf0
(d) \par
}
{\phpg\posx2796\pvpg\posy12017\absw308\absh1481 \f10 \fs18 \cf0 \f10 \fs18 \cf0
(e)
\par}{\phpg\posx2796\pvpg\posy12017\absw308\absh1481 \sl-314 \f10 \fs18 \cf0 (f)
\par}{\phpg\posx2796\pvpg\posy12017\absw308\absh1481 \sl-275 \par\f10 \fs18 \cf0
(g)
\par}{\phpg\posx2796\pvpg\posy12017\absw308\absh1481 \sl-275 \par\f10 \fs18 \cf0
(h) \par
}
{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \f10 \fs18 \cf0 \f10 \fs18 \cf0
Campur contoh uji dan pindahkan sejumLah volume yang sesuai (50 mL
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-238 \f10 \fs18 \cf0 sam
pai dengan 100 mL) ke dalam labu alas bulat atau erlenmeyer 125 mL.
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-170 \par\f10 \fs18 \cf0
Tambahkan 5 mL HNO{\dn006 \fs11 3} pekat dan beberapa batu didih atau butiran
gelas.
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-285 \f10 \fs18 \cf0 Did
ihkan perlahan-lahan dan uapkan pada{\i hot}{\i plate} hingga volume
contoh uji
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-237 \f10 \fs18 \cf0 men
jadi yang mungkin kira-kira 10 mL -20 mL.
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-170 \par\f10 \fs18 \cf0
Lanjutkan pemanasan dan tambahkan HNO{\dn006 \fs11 3} pekat sesuai kepe
rluan hingga
\par}{\phpg\posx3303\pvpg\posy9812\absw7712\absh3465 \sl-209 \f10 \fs18 \cf0 dig
esti sempurna yang terlihat dari larutan jernih-berwarna. Hindari contoh
uji
}
{\phpg\posx2251\pvpg\posy2539\absw1042\absh1428 \f20 \fs20 \cf0 \f20 \fs20 \cf0
V{\fs17 C }{\fs17 .}{\fs17 u}{\fs17 . }
\par}{\phpg\posx2251\pvpg\posy2539\absw1042\absh1428 \sl-367 \f20 \fs20 \cf0 {\f
s20 V}{\fs16 EDTA}{\f40 \fs22 (}{\fs16 a}{\f40 \fs22 ) }
\par}{\phpg\posx2251\pvpg\posy2539\absw1042\absh1428 \sl-292 \par\f20 \fs20 \cf0
{\fs20 M}{\dn006 \fs16 EDTA }
\par}{\phpg\posx2251\pvpg\posy2539\absw1042\absh1428 \sl-320 \f20 \fs20 \cf0 {\d
n006 \fs20 V}{\fs17 EDTA}{\f40 \fs23 [}{\fs17 b}{\f40 \fs23 ] }\par
}
{\phpg\posx3404\pvpg\posy2521\absw705\absh1353 \f10 \fs18 \cf0 \f10 \fs18 \cf0 a
dalah
\par}{\phpg\posx3404\pvpg\posy2521\absw705\absh1353 \sl-338 \f10 \fs18 \cf0 adal
ah
\par}{\phpg\posx3404\pvpg\posy2521\absw705\absh1353 \sl-307 \par\f10 \fs18 \cf0
adalah
\par}{\phpg\posx3404\pvpg\posy2521\absw705\absh1353 \sl-320 \f10 \fs18 \cf0 adal
ah \par
}
{\phpg\posx4759\pvpg\posy1615\absw561\absh554 \f20 \fs20 \cf0 \fi22 \f20 \fs20 \
cf0 1000
\par}{\phpg\posx4759\pvpg\posy1615\absw561\absh554 \sl-187 \par\f20 \fs20 \cf0 V
{\fs17 C }{\fs17 .}{\fs17 u}{\fs17 . }\par
}
{\phpg\posx5331\pvpg\posy1757\absw1186\absh279 \f20 \fs20 \cf0 \f20 \fs20 \cf0 x
V
\par}{\phpg\posx5331\pvpg\posy1757\absw1186\absh279 \sl-224 \f20 \fs20 \cf0 \fi3
34 {\fs17 EDTA}{\f40 \fs22 (}{\fs17 b}{\f40 \fs22 ) }\par
}
{\phpg\posx6483\pvpg\posy1757\absw436\absh225 \f20 \fs20 \cf0 \f20 \fs20 \cf0 x
M \par
}
{\phpg\posx6886\pvpg\posy1757\absw1001\absh276 \f20 \fs17 \cf0 \f20 \fs17 \cf0 E
DTA{\fs20 x}{\fs20 40 }\par
}
{\phpg\posx4249\pvpg\posy2521\absw6299\absh1392 \f10 \fs18 \cf0 \f10 \fs18 \cf0
volume larutan contoh uji (mL)
\par}{\phpg\posx4249\pvpg\posy2521\absw6299\absh1392 \sl-183 \par\f10 \fs18 \cf0
volume rata-rata larutan baku Na{\dn006 \fs11 2}EDTA untuk titrasi kesa
dahan
\par}{\phpg\posx4249\pvpg\posy2521\absw6299\absh1392 \sl-209 \f10 \fs18 \cf0 tot
al (mL).
\par}{\phpg\posx4249\pvpg\posy2521\absw6299\absh1392 \sl-202 \par\f10 \fs18 \cf0
molaritas larutan baku Na{\dn006 \fs11 2}EDTA untuk titrasi (mmol/mL).
\par}{\phpg\posx4249\pvpg\posy2521\absw6299\absh1392 \sl-320 \f10 \fs18 \cf0 vol
ume rata-rata larutan baku Na{\dn006 \fs11 2}EDTA untuk titrasi kalsium (mL) \p
ar
}
{\phpg\posx2117\pvpg\posy4389\absw7102\absh636 \b \f10 \fs18 \cf0 \b \f10 \fs18
\cf0 3.7.2
Persen temu balik{\b0 (%}{\b0\i Recovery}{\b0 ,}{\b0 %}{\b0 R)
}
\par}{\phpg\posx2117\pvpg\posy4389\absw7102\absh636 \sl-238 \par\b \f10 \fs18 \c
f0 {\b0 Persen}{\b0 temu}{\b0 balik}{\b0 dihitung}{\b0 dengan}{\b0 mengguna
kan}{\b0 rumus}{\b0 sebagai}{\b0 berikut}{\b0 : }\par
}
{\phpg\posx3165\pvpg\posy5466\absw653\absh249 \f20 \fs20 \cf0 \f20 \fs20 \cf0 %
R{\f40 = }\par
}
{\phpg\posx3810\pvpg\posy5324\absw575\absh535 \f20 \fs20 \cf0 \f20 \fs20 \cf0 A{
\f40 {\field{\*\fldinst SYMBOL 45 \\f Symbol }}} B
\par
}
{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \f10 \fs18 \cf0 \f10 \fs18 \cf0
Gunakan bahan kimia berderajat pro analisis (p.a.).
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-314 \f10 \fs18 \cf0 Gu
nakan alat gelas bebas kontaminan.
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-311 \f10 \fs18 \cf0 Gu
nakan alat ukur yang terkalibrasi atau terverifikasi.
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-314 \f10 \fs18 \cf0 Gu
nakan air suling untuk pembuatan semua pereaksi dan larutan kerja.
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-313 \f10 \fs18 \cf0 Di
kerjakan oleh analis/penguji yang berkompeten.
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-311 \f10 \fs18 \cf0 La
kukan uji dalam jangka waktu yang tidak melampaui waktu simpan maksimu
m
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-238 \f10 \fs18 \cf0 ({
\i holding}{\i time}) yaitu 6 bulan setelah diasamkan dengan asam nitrat hingga
pH kurang
\par}{\phpg\posx2651\pvpg\posy11314\absw8398\absh2045 \sl-237 \f10 \fs18 \cf0 da
ri 2. \par
}
{\phpg\posx6057\pvpg\posy14932\absw692\absh189 \f10 \fs17 \cf0 \f10 \fs17 \cf0 6
{\b dari}{\b 8 }\par
}
{\shp\shpfhdr0\shpbxpage\shpbypage\shpfblwtxt1\shpz0
\shpleft3277\shptop8422\shpright3925\shpbottom8422
{\*\shpinst {\sp{\sn shapeType}{\sv 20}}
{\sp{\sn fFlipH}{\sv 0}}{\sp{\sn fFlipV}{\sv 0}}
{\sp{\sn LineWidth}{\sv
9}}
{\sp{\sn fBehindDocument}{\sv 1}}{\sp{\sn lineColor}{\sv
0}}}}
\sect\sectd\pard\plain
\pgwsxn12240\pghsxn15840
{\phpg\posx8676\pvpg\posy806\absw2082\absh207 \b \f10 \fs18 \cf0 \b \f10 \fs18 \
cf0 SNI 06-6989.13-2004 \par
}
{\phpg\posx2118\pvpg\posy1628\absw8575\absh706 \b \f10 \fs18 \cf0 \b \f10 \fs18
\cf0 4.2
Pengendalian mutu
\par}{\phpg\posx2118\pvpg\posy1628\absw8575\absh706 \sl-252 \par\b \f10 \fs18 \c
f0 {\b0 Lakukan}{\b0 uji}{\b0 secara}{\b0 duplo}{\b0 untuk}{\b0 kontrol}{\b
0 ketelitian.}{\b0 Perbedaan}{\b0 pemakaian}{\b0 larutan}{\b0 Na}{\b0\dn006
\fs11 2}{\b0 EDTA }\par
}
{\phpg\posx2118\pvpg\posy2341\absw4794\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 s
ecara duplo tidak boleh lebih besar dari 0,10 mL. \par
}
{\phpg\posx2118\pvpg\posy3056\absw146\absh207 \b \f10 \fs18 \cf0 \b \f10 \fs18 \
cf0 5 \par
}
{\phpg\posx2626\pvpg\posy3056\absw1440\absh207 \b \f10 \fs18 \cf0 \b \f10 \fs18
\cf0 Rekomendasi \par
}
{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \f10 \fs18 \cf0 \f10 \fs18 \cf0
Lakukan kontrol akursi dengan salah satu cara dibawah ini:
\par}{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \sl-238 \par\f10 \fs18 \cf0
a)
Analisis CRM
\par}{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \sl-313 \f10 \fs18 \cf0 \fi
400 Lakukan analisis{\i Certified}{\i Reference}{\i Material} (CRM) unt
uk kontrol akurasi. Larutan
\par}{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \sl-237 \f10 \fs18 \cf0 \fi
400 pekat CRM diencerkan dengan air suling sampai konsentrasi 1,0 mg/L.
Kemudian
\par}{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \sl-238 \f10 \fs18 \cf0 \fi
400 lakukan langkah 3.5 b) dan 3.5.g) dari 3.5.
\par}{\phpg\posx2118\pvpg\posy3531\absw8930\absh1627 \sl-311 \f10 \fs18 \cf0 b)
Lakukan uji{\i blind}{\i sample. }\par
}
{\phpg\posx2118\pvpg\posy5424\absw228\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 c)
\par
}
{\phpg\posx2518\pvpg\posy5424\absw8520\absh421 \f10 \fs18 \cf0 \f10 \fs18 \cf0 K
isaran persen temu balik adalah 85% sampai dengan 115% atau sesuai de
ngan
\par}{\phpg\posx2518\pvpg\posy5424\absw8520\absh421 \sl-237 \f10 \fs18 \cf0 krit
eria dalam sertifikat CRM. \par
}
{\phpg\posx2118\pvpg\posy5974\absw8939\absh703 \f10 \fs18 \cf0 \f10 \fs18 \cf0 d
)
Untuk kontrol gangguan matriks lakukan uji{\i spike}{\i matrix}.
Kisaran persen temu balik
\par}{\phpg\posx2118\pvpg\posy5974\absw8939\absh703 \sl-238 \f10 \fs18 \cf0 \fi4
00 adalah 85% sampai dengan 115%.
\par}{\phpg\posx2118\pvpg\posy5974\absw8939\absh703 \sl-311 \f10 \fs18 \cf0 e)
Buat kartu kendali ({\i control}{\i chart}) untuk akurasi pengujian. \par
}
{\phpg\posx6057\pvpg\posy14932\absw694\absh189 \b \f10 \fs17 \cf0 \b \f10 \fs17
\cf0 7 dari 8 \par
}
\sect\sectd\pard\plain
\pgwsxn12240\pghsxn15840
{\phpg\posx2118\pvpg\posy806\absw2082\absh207 \b \f10 \fs18 \cf0 \b \f10 \fs18 \
cf0 SNI 06-6989.13-2004 \par
}
{\phpg\posx5764\pvpg\posy1607\absw1322\absh876 \b \f10 \fs20 \cf0 \b \f10 \fs20
\cf0 Lampiran A
\par}{\phpg\posx5764\pvpg\posy1607\absw1322\absh876 \sl-353 \b \f10 \fs20 \cf0 \
fi127 {\b0 \fs18 (informatif) }
\par}{\phpg\posx5764\pvpg\posy1607\absw1322\absh876 \sl-368 \b \f10 \fs20 \cf0 \
fi75 Pelaporan \par
}
{\phpg\posx2118\pvpg\posy3303\absw4394\absh207 \f10 \fs18 \cf0 \f10 \fs18 \cf0 C
atat pada buku kerja hal-hal sebagai berikut: \par
}
{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \f10 \fs18 \cf0 \f10 \fs18 \cf0 1
)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-314 \f10 \fs18 \cf0 2)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-311 \f10 \fs18 \cf0 3)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-314 \f10 \fs18 \cf0 4)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-313 \f10 \fs18 \cf0 5)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-313 \f10 \fs18 \cf0 6)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-313 \f10 \fs18 \cf0 7)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-313 \f10 \fs18 \cf0 8)
\par}{\phpg\posx2118\pvpg\posy3779\absw228\absh2463 \sl-313 \f10 \fs18 \cf0 9) \
par
}
{\phpg\posx2626\pvpg\posy3779\absw3065\absh2463 \f10 \fs18 \cf0 \f10 \fs18 \cf0
Parameter yang dianalisis.
\par}{\phpg\posx2626\pvpg\posy3779\absw3065\absh2463 \sl-314 \f10 \fs18 \cf0 Nam
a dan tanda tangan/ analis.
\par}{\phpg\posx2626\pvpg\posy3779\absw3065\absh2463 \sl-311 \f10 \fs18 \cf0 Tan
ggal analisis.
\par}{\phpg\posx2626\pvpg\posy3779\absw3065\absh2463 \sl-314 \f10 \fs18 \cf0 Rek